CN112345482A - Analysis method for carbon content in aluminum material - Google Patents
Analysis method for carbon content in aluminum material Download PDFInfo
- Publication number
- CN112345482A CN112345482A CN202011146711.1A CN202011146711A CN112345482A CN 112345482 A CN112345482 A CN 112345482A CN 202011146711 A CN202011146711 A CN 202011146711A CN 112345482 A CN112345482 A CN 112345482A
- Authority
- CN
- China
- Prior art keywords
- aluminum material
- detected
- washing
- fluxing agent
- pickling
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 129
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000000463 material Substances 0.000 title claims abstract description 122
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000004458 analytical method Methods 0.000 title claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 73
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 49
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 42
- AWXLLPFZAKTUCQ-UHFFFAOYSA-N [Sn].[W] Chemical compound [Sn].[W] AWXLLPFZAKTUCQ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000010521 absorption reaction Methods 0.000 claims abstract description 31
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 claims abstract description 21
- 238000005554 pickling Methods 0.000 claims description 54
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 44
- 239000007787 solid Substances 0.000 claims description 36
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 230000004907 flux Effects 0.000 claims description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims description 22
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 claims description 14
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 13
- 238000007603 infrared drying Methods 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052721 tungsten Inorganic materials 0.000 claims description 10
- 239000010937 tungsten Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000002604 ultrasonography Methods 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 6
- 238000001514 detection method Methods 0.000 description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000010425 asbestos Substances 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052895 riebeckite Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- HLLSOEKIMZEGFV-UHFFFAOYSA-N 4-(dibutylsulfamoyl)benzoic acid Chemical group CCCCN(CCCC)S(=O)(=O)C1=CC=C(C(O)=O)C=C1 HLLSOEKIMZEGFV-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000002311 subsequent effect Effects 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- 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
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
- G01N21/274—Calibration, base line adjustment, drift correction
- G01N21/278—Constitution of standards
Landscapes
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Mathematical Physics (AREA)
- Theoretical Computer Science (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention provides an analysis method for carbon content in an aluminum material, which comprises the following steps: (1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying to obtain a pretreated aluminum material; (2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method; the fluxing agent used by the infrared absorption method is a combination of a pure iron fluxing agent and a tungsten-tin fluxing agent. The invention can stably detect the high-purity aluminum material with the carbon content within the range of 1-10ppm by pre-treating the aluminum material to be detected and selecting the specific fluxing agent when the analysis method is used for detecting the carbon content in the high-purity aluminum material.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and relates to a method for analyzing carbon content, in particular to a method for analyzing carbon content in an aluminum material.
Background
The technology in the semiconductor industry is rapidly developed, the number of input/output leads inside integrated circuits and microprocessor chips is rapidly increased, the length of interconnection lines and the density of the interconnection lines are continuously increased, and meanwhile, the sectional area of the interconnection lines and the distance between the interconnection lines are continuously reduced, so that the technical requirements of the semiconductor industry on metal interconnection lines are continuously increased.
The aluminum material, especially the high-purity aluminum (the purity is more than or equal to 5N) target material is a main material for manufacturing the metal interconnection line, and has the advantages of high conductivity, easy processing, easy deposition and easy photoetching; and the electrochemical corrosion resistance is strong, and the cost is relatively low, so the method is widely applied to the physical vapor deposition sputtering coating process.
However, the high-purity aluminum target has small density, and when the high-purity aluminum target is bombarded by high-voltage electrons, elements such as carbon, oxygen, nitrogen, hydrogen and the like contained in the defects in the high-purity aluminum target are released, so that target particles are easy to splash, the quality of the film is greatly reduced, and the metal interconnection line is short-circuited. Therefore, it is important to accurately measure the contents of carbon, oxygen, nitrogen and hydrogen elements in the high-purity aluminum target.
CN 103245633A discloses a method for determining carbon and sulfur contents in rare earth aluminum alloy by using a heterostandard correction infrared absorption method, wherein an alloy is selected as a first standard sample according to the carbon and sulfur contents of a rare earth aluminum alloy sample; two alloys are alternatively used as a second standard sample and a third standard sample; determining the contents of carbon and sulfur in the fluxing agent as blank values, and inputting the blank values into an infrared carbon and sulfur determinator; respectively introducing the first standard sample, the second standard sample and the third standard sample into an infrared carbon-sulfur tester after inputting a blank value for analysis, and correcting a working curve of the infrared carbon-sulfur tester; and introducing the rare earth aluminum alloy sample into a corrected infrared carbon-sulfur determinator for measurement to respectively obtain the carbon content and the sulfur content in the rare earth aluminum alloy sample.
However, besides the standard curve, each link in the infrared absorption method affects the measurement result. Such as oxygen flow, crucible pretreatment, and sample pretreatment.
CN 105842182a discloses a method for determining the content of free carbon in a covering agent, comprising the following steps: (1) and (3) linearization correction: respectively weighing barium carbonate reference substances with different amounts, burning the barium carbonate reference substances, and mixingSpreading pure iron fluxing agent in a crucible, and analyzing the crucible as a carbon standard series in an infrared carbon-sulfur analyzer, and performing instrument linearization correction; (2) determination of the carbon content in the covering agent: pulverizing the covering agent, drying, dissolving with acid, and boiling to remove carbon dioxide; adding the covering agent solution into a funnel paved with calcined acid-washed asbestos soaked in high-purity water for vacuum filtration, draining off water, taking out the acid-washed asbestos with precipitate, placing the acid-washed asbestos with precipitate into an infrared special crucible which is calcined and paved with pure iron fluxing agent and tin fluxing agent, drying, placing the crucible into an infrared carbon-sulfur analyzer for determination, and converting carbon into CO under the action of the fluxing agent and oxygen2Desulfurization, introduction of CO2And (5) an infrared absorption cell for measuring the carbon content.
However, the pure iron flux and the tin flux are difficult to be fully combusted, so that blank control data of the flux is large in fluctuation, and the high-purity aluminum target material with the carbon content of less than 10ppm is difficult to detect by using the method.
Aiming at the defects of the prior art, the invention provides a simple and feasible analysis method, which can stably detect a high-purity aluminum target sample with carbon content in the range of 1-10ppm by pretreating the detected high-purity aluminum target and selecting a specific fluxing agent composition and a fluxing agent adding proportion.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an analysis method for the carbon content in an aluminum material, and particularly relates to an analysis method for the carbon content in a high-purity aluminum material. The analysis method can stably detect the high-purity aluminum material with the carbon content of 1-10ppm, thereby overcoming the problem that the prior art can not detect the sample with the carbon content less than 10 ppm.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an analysis method for carbon content in an aluminum material, which comprises the following steps:
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying to obtain a pretreated aluminum material;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method; the fluxing agent used by the infrared absorption method is a combination of a pure iron fluxing agent and a tungsten-tin fluxing agent.
According to the invention, firstly, the aluminum material to be detected is subjected to acid washing, water washing and acetone washing in sequence, and then dried to obtain the pretreated aluminum material, so that adverse effects of impurities on the surface of the aluminum material to be detected on detection are effectively avoided, and the detection accuracy is effectively improved; and then, selecting a fluxing agent in an infrared absorption method to ensure that the aluminum material to be detected and the fluxing agent can be fully combusted, wherein the fluxing agent consisting of the pure iron fluxing agent and the tungsten tin fluxing agent can be fully combusted during blank value calibration, and the obtained blank value is relatively stable, so that the detection limit and the detection stability of the analysis method are improved.
Preferably, the aluminum material to be detected in the step (1) is a high-purity aluminum material; the purity of the high-purity aluminum material is more than or equal to 5N.
Preferably, the pickling solution used in the pickling in the step (1) is formed by mixing hydrofluoric acid, nitric acid and deionized water.
Preferably, the volume ratio of the hydrofluoric acid to the nitric acid to the deionized water is (1-2) to (6-8), and the volume ratio can be, for example, 1:1:6, 1:1:7, 1:1:8, 1:2:6, 2:1:6, 1:2:7, 2:1:7, 1:2:8, 2:2:6, 2:2:7 or 2:2:8, but is not limited to the enumerated values, and other unrecited values in the numerical range can be equally applicable; preferably 1:1: 6.
Preferably, the concentration of hydrofluoric acid is 35-40 wt.%, for example 35 wt.%, 36 wt.%, 37 wt.%, 38 wt.%, 39 wt.% or 40 wt.%, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the nitric acid has a concentration of 65 to 70 wt.%, for example 65 wt.%, 66 wt.%, 67 wt.%, 68 wt.%, 69 wt.% or 70 wt.%, but is not limited to the recited values, and other values not recited within the numerical range are equally applicable.
Preferably, the number of acid washing steps (1) is at least 3, such as 3, 4, 5, 6, 7 or 8, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the time per pickling is at least 1min, and may be, for example, 1min, 2min, 3min, 4min, 5min or 6min, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the ratio of the amount of the pickling solution used per pickling to the liquid-solid ratio of the aluminum material to be tested is (5-10):1, and can be, for example, 5:1, 6:1, 7:1, 8:1, 9:1 or 10:1, but is not limited to the values listed, and other values not listed in the numerical range are also applicable, and the unit of the liquid-solid ratio is mg/L.
Preferably, the number of times of water washing in step (1) is at least 3, for example, 3, 4, 5, 6, 7, 8 or 10 times, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the time of each water wash is at least 2min, for example, 2min, 4min, 6min, 8min or 10min, but is not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the ratio of the amount of the deionized water to the liquid to solid of the aluminum material to be detected in each water washing is (5-10):1, for example, 5:1, 6:1, 7:1, 8:1, 9:1 or 10:1, but the method is not limited to the enumerated values, and other unrecited values in the numerical range are also applicable, and the unit of the liquid to solid ratio is mg/L.
Preferably, the water washing of step (1) is accompanied by ultrasound.
The acid washing can effectively remove impurities on the surface of the aluminum material to be detected through corrosion, but acid residues easily exist, and the later period is not favorable for measuring the carbon content in the aluminum material to be detected. The invention can effectively reduce the acid residue by washing with water under the ultrasonic condition, thereby ensuring the detection limit and stability of the infrared absorption method.
Preferably, the drying in step (1) is drying by using an infrared drying lamp.
According to the invention, the infrared drying lamp is selected to dry the aluminum material to be detected, so that impurities carried by a heat exchange medium are effectively avoided, and the detection limit and stability of infrared absorption method detection are ensured in the drying stage.
Preferably, the mass ratio of the tungsten-tin flux to the pure iron flux in step (2) is (1.2-1.6):1, and may be, for example, 1.2:1, 1.3:1, 1.4:1, 1.5:1 or 1.6:1, but is not limited to the recited values, and ranges of values other than the recited values are equally applicable.
Preferably, the mass percent of tin in the tungsten-tin flux is 12-21%, and the balance is tungsten and inevitable impurities.
The mass percent of tin in the tungsten-tin flux is 12-21%, and may be, for example, 12%, 14%, 15%, 16%, 18%, 20%, or 21%, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the C in the tungsten-tin fluxing agent is less than or equal to 6ppm, and the S is less than or equal to 6 ppm.
According to the invention, the specific composition of the tungsten-tin fluxing agent and the proportion of the pure iron fluxing agent to the tungsten-tin fluxing agent are selected, so that the fluxing agent can be completely combusted during blank value calibration, and the obtained calibration blank value is stable and accurate. And the fluxing agent can ensure that the aluminum material to be detected is completely combusted, so that the detection limit and the stability of the infrared absorption method detection are ensured.
Preferably, the analysis method further comprises a pre-treatment step prior to step (1): and (3) sequentially crushing and screening the aluminum material to be detected, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1).
As a preferable technical scheme, the aluminum material to be detected with the granularity of 20-50 meshes is selected by crushing and screening, so that the subsequent effects of acid washing, water washing, acetone washing and drying are ensured, the determination time of an infrared absorption method is shortened, and the influence of external factors on the accuracy of a detection result is reduced to a certain extent.
Preferably, the infrared absorption method of step (2) is performed in a LECO CS844 carbon sulfur analyzer.
As a preferred embodiment of the present invention, there is provided an analysis method comprising the steps of:
pretreatment: sequentially crushing and screening the aluminum material to be detected with the purity of more than or equal to 5N, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1);
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying by using an infrared drying lamp to obtain a pretreated aluminum material; the pickling solution for pickling is formed by mixing hydrofluoric acid, nitric acid and deionized water according to the volume ratio of (1-2) to (6-8), wherein the concentration of the hydrofluoric acid is 35-40 wt%, and the concentration of the nitric acid is 65-70 wt%;
the number of pickling times is at least 3, the pickling time is at least 1min, the ratio of the consumption of pickling solution to the liquid-solid ratio of the aluminum material to be detected in each pickling process is (5-10):1, and the unit of the liquid-solid ratio is mg/L;
the washing times are at least 3, the washing time is at least 2min, the ratio of the consumption of deionized water to the liquid-solid ratio of the aluminum material to be detected in each washing is (5-10):1, and the unit of the liquid-solid ratio is mg/L; the water washing is accompanied by ultrasound;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method; the fluxing agent used by the infrared absorption method is a combination of tungsten tin fluxing agent and pure iron fluxing agent in a mass ratio of (1.2-1.6) to 1;
the mass percent of tin in the tungsten-tin fluxing agent is 12-21%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
the invention can stably detect the high-purity aluminum material with the carbon content within the range of 1-10ppm by pre-treating the aluminum material to be detected and selecting the specific fluxing agent when the analysis method is used for detecting the carbon content in the high-purity aluminum material.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
The embodiment provides an analysis method for carbon content in a high-purity aluminum material, which comprises the following steps:
pretreatment: sequentially crushing and screening the aluminum material to be detected with the purity of 5N, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1);
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying by using an infrared drying lamp to obtain a pretreated aluminum material; the pickling solution for pickling is formed by mixing hydrofluoric acid, nitric acid and deionized water in a volume ratio of 1:1:6, wherein the concentration of the hydrofluoric acid is 35 wt%, and the concentration of the nitric acid is 70 wt%;
the pickling frequency is 3 times, the pickling time is 1min, the using amount of pickling solution and the liquid-solid ratio of the aluminum material to be detected are 8:1 during each pickling, and the unit of the liquid-solid ratio is mg/L;
the washing times are 3 times, the washing time is 2min, the ratio of the consumption of deionized water to the liquid-solid ratio of the aluminum material to be detected is 8:1, and the unit of the liquid-solid ratio is mg/L; the water washing is accompanied by ultrasound;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method in an LECO CS844 carbon-sulfur analyzer; the fluxing agent used by the infrared absorption method is a combination of a tungsten-tin fluxing agent and a pure iron fluxing agent in a mass ratio of 1.4: 1;
the mass percent of tin in the tungsten-tin fluxing agent is 16%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
Example 2
The embodiment provides an analysis method for carbon content in a high-purity aluminum material, which comprises the following steps:
pretreatment: sequentially crushing and screening the aluminum material to be detected with the purity of 5N, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1);
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying by using an infrared drying lamp to obtain a pretreated aluminum material; the pickling solution for pickling is formed by mixing hydrofluoric acid, nitric acid and deionized water in a volume ratio of 1:1:7, wherein the concentration of the hydrofluoric acid is 36 wt%, and the concentration of the nitric acid is 69 wt%;
the acid washing times are 4 times, the time of each acid washing is 2min, the ratio of the consumption of the acid washing liquid to the liquid-solid ratio of the aluminum material to be detected is 6:1, and the unit of the liquid-solid ratio is mg/L;
the washing times are 4 times, the washing time is 4min, the ratio of the amount of deionized water to the liquid-solid ratio of the aluminum material to be detected is 6:1, and the unit of the liquid-solid ratio is mg/L; the water washing is accompanied by ultrasound;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method in an LECO CS844 carbon-sulfur analyzer; the fluxing agent used by the infrared absorption method is a combination of a tungsten-tin fluxing agent and a pure iron fluxing agent in a mass ratio of 1.3: 1;
the mass percent of tin in the tungsten-tin fluxing agent is 18%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
Example 3
The embodiment provides an analysis method for carbon content in a high-purity aluminum material, which comprises the following steps:
pretreatment: sequentially crushing and screening the aluminum material to be detected with the purity of 5N, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1);
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying by using an infrared drying lamp to obtain a pretreated aluminum material; the pickling solution for pickling is formed by mixing hydrofluoric acid, nitric acid and deionized water in a volume ratio of 1:1:8, wherein the concentration of the hydrofluoric acid is 38 wt%, and the concentration of the nitric acid is 68 wt%;
the pickling frequency is 5 times, the pickling time is 1min, the using amount of pickling solution and the liquid-solid ratio of the aluminum material to be detected are 5:1 during each pickling, and the unit of the liquid-solid ratio is mg/L;
the washing times are 5 times, the washing time is 2min, the ratio of the consumption of deionized water to the liquid-solid ratio of the aluminum material to be detected is 5:1, and the unit of the liquid-solid ratio is mg/L; the water washing is accompanied by ultrasound;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method in an LECO CS844 carbon-sulfur analyzer; the fluxing agent used by the infrared absorption method is a combination of a tungsten-tin fluxing agent and a pure iron fluxing agent in a mass ratio of 1.5: 1;
the mass percent of tin in the tungsten-tin fluxing agent is 14%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
Example 4
The embodiment provides an analysis method for carbon content in a high-purity aluminum material, which comprises the following steps:
pretreatment: sequentially crushing and screening the aluminum material to be detected with the purity of 5N, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1);
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying by using an infrared drying lamp to obtain a pretreated aluminum material; the pickling solution for pickling is formed by mixing hydrofluoric acid, nitric acid and deionized water in a volume ratio of 2:2:7, wherein the concentration of the hydrofluoric acid is 39 wt%, and the concentration of the nitric acid is 66 wt%;
the pickling frequency is 3 times, the pickling time is 3min, the using amount of pickling solution and the liquid-solid ratio of the aluminum material to be detected in each pickling process are 9:1, and the unit of the liquid-solid ratio is mg/L;
the washing times are 3 times, the washing time is 6min, the ratio of the consumption of deionized water to the liquid-solid ratio of the aluminum material to be detected is 9:1, and the unit of the liquid-solid ratio is mg/L; the water washing is accompanied by ultrasound;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method in an LECO CS844 carbon-sulfur analyzer; the fluxing agent used by the infrared absorption method is a combination of a tungsten-tin fluxing agent and a pure iron fluxing agent in a mass ratio of 1.2: 1;
the mass percent of tin in the tungsten-tin fluxing agent is 21%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
Example 5
The embodiment provides an analysis method for carbon content in a high-purity aluminum material, which comprises the following steps:
pretreatment: sequentially crushing and screening the aluminum material to be detected with the purity of 5N, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1);
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying by using an infrared drying lamp to obtain a pretreated aluminum material; the pickling solution for pickling is formed by mixing hydrofluoric acid, nitric acid and deionized water in a volume ratio of 2:2:8, wherein the concentration of the hydrofluoric acid is 40 wt%, and the concentration of the nitric acid is 65 wt%;
the pickling frequency is 3 times, the pickling time is 3min, the using amount of pickling solution and the liquid-solid ratio of the aluminum material to be detected in each pickling process are 10:1, and the unit of the liquid-solid ratio is mg/L;
the washing times are 3 times, the washing time is 6min, the ratio of the consumption of deionized water to the liquid-solid ratio of the aluminum material to be detected is 10:1, and the unit of the liquid-solid ratio is mg/L; the water washing is accompanied by ultrasound;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method in an LECO CS844 carbon-sulfur analyzer; the fluxing agent used by the infrared absorption method is a combination of a tungsten-tin fluxing agent and a pure iron fluxing agent in a mass ratio of 1.6: 1;
the mass percent of tin in the tungsten-tin fluxing agent is 12%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
Example 6
This example provides a method for analyzing the carbon content in a high purity aluminum material, which is the same as example 1 except that the pickling solution used in step (1) is prepared by mixing hydrofluoric acid and deionized water in a volume ratio of 1: 7.
Example 7
This example provides a method for analyzing the carbon content in a high purity aluminum material, which is the same as example 1 except that the pickling solution used in step (1) is a mixture of nitric acid and deionized water in a volume ratio of 1: 7.
Example 8
The embodiment provides a method for analyzing the carbon content in a high-purity aluminum material, which is the same as the embodiment 1 except that the drying in the step (1) is the hot air drying for removing carbon dioxide.
Example 9
This example provides a method for analyzing the carbon content in a high purity aluminum material, which is the same as that in example 1 except that the mass ratio of the tungsten-tin flux to the pure iron flux in step (2) is 1: 1.
Example 10
This example provides a method for analyzing the carbon content in a high purity aluminum material, which is the same as that of example 1 except that the mass ratio of the tungsten-tin flux to the pure iron flux in step (2) is 1.8: 1.
Comparative example 1
This comparative example provides a method for analyzing the carbon content in a high purity aluminum material, which was the same as in example 1 except that the water washing in step (1) was not performed.
Comparative example 2
This comparative example provides a method for analyzing the carbon content in a high purity aluminum material, which is the same as that of example 1 except that the flux in step (2) is a pure iron flux.
Comparative example 3
The comparative example provides a method for analyzing the carbon content in the high-purity aluminum material, which is the same as that in example 1 except that the fluxing agent in the step (2) is a tungsten-tin fluxing agent.
The mass percent of tin in the tungsten-tin fluxing agent is 16%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
The high-purity aluminum materials tested in examples 1-10 and comparative examples 1-3 of the invention are high-purity aluminum materials of the same batch, namely, the same high-purity aluminum material is crushed and sieved, the high-purity aluminum material sample which is sieved by a 20-mesh sieve but not sieved by a 50-mesh sieve is divided into 14 parts, and the part which is not pretreated is used as a blank control.
When the infrared absorption method is used for measurement, the crucible is burnt in a muffle furnace at 1200 ℃ for 4 hours; the purity of the used oxygen is 5N, the oxygen is pretreated before use to remove impurities such as carbon monoxide, methane, carbon dioxide and the like contained in the oxygen, and the oxygen is dehumidified by magnesium perchlorate and then introduced into an LECO CS844 carbon-sulfur analyzer.
When carbon content was measured using a LECO CS844 carbon sulfur analyzer, NaOH was used as CO2An absorbent; the instrument parameters are set as follows: the power voltage is 220V, the pre-cleaning time is 10s, the shortest analysis time of C is 35s, and the compensation comparison level of C is 2%. The analysis results of examples 1 to 10 and comparative examples 1 to 3 are shown in Table 1.
TABLE 1
As can be seen from Table 1, the analysis methods provided in examples 1 to 5 of the present invention all can obtain a carbon content of 1 to 10ppm in the high purity aluminum material, and the detection results have small fluctuation.
In example 6, nitric acid was not added during pickling, and the pickling effect was not good, and the result of measuring the carbon content of the high purity aluminum material (purity 5N) was 28ppm, and the distortion of the result was serious. In example 7, hydrofluoric acid was not added during the pickling, and the pickling effect was not good, and the result of measuring the carbon content of the high purity aluminum material (purity 5N) reached 43ppm, and the obtained result was distorted significantly.
In example 8, hot air for removing carbon dioxide is selected for drying during drying, but the amount of hot air used for drying is large, the effect of removing carbon dioxide is difficult to ensure, and the result of measuring the carbon content of the high-purity aluminum material (with the purity of 5N) reaches 37ppm finally.
In examples 9 and 10, the mass ratio of the tungsten-tin flux to the pure iron flux was 1:1 and 1.8:1, respectively, and the flux exhibited a flux action, but the flux itself was not sufficiently combusted, and the blank was unstable, and the results were shifted to 12ppm and 11ppm, respectively.
In comparative example 1, water washing was not performed, and it was difficult to overcome the adverse effect of the acid solution used in acid washing on the subsequent detection. The final test results deviated to 33 ppm. In comparative examples 2 and 3, a single flux was used, the flux effect was poor, the blank was unstable, and the results were deviated to 14ppm and 16ppm, respectively.
In summary, the invention enables the analysis method to stably detect the high-purity aluminum material with the carbon content in the range of 1-10ppm when detecting the carbon content in the high-purity aluminum material by pre-treating the aluminum material to be detected and selecting the specific fluxing agent.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An analysis method for carbon content in an aluminum material, characterized by comprising the steps of:
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying to obtain a pretreated aluminum material;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method; the fluxing agent used by the infrared absorption method is a combination of a pure iron fluxing agent and a tungsten-tin fluxing agent.
2. The analysis method according to claim 1, wherein the aluminum material to be tested in the step (1) is a high-purity aluminum material; the purity of the high-purity aluminum material is more than or equal to 5N.
3. The analytical method according to claim 1 or 2, wherein the pickling solution used in the pickling in the step (1) is a mixture of hydrofluoric acid, nitric acid and deionized water;
preferably, the volume ratio of the hydrofluoric acid to the nitric acid to the deionized water is (1-2) to (6-8), and preferably 1:1: 6;
preferably, the concentration of the hydrofluoric acid is 35-40 wt%;
preferably, the concentration of the nitric acid is 65 to 70 wt%.
4. The assay of claim 3, wherein the number of acid washes of step (1) is at least 3;
preferably, the time of each pickling is at least 1 min;
preferably, the ratio of the amount of the pickling solution to the liquid-solid ratio of the aluminum material to be detected in each pickling is (5-10):1, and the unit of the liquid-solid ratio is mg/L.
5. The assay of any one of claims 1-4, wherein the number of water washes of step (1) is at least 3;
preferably, the time of each water wash is at least 2 min;
preferably, the ratio of the amount of deionized water to the liquid to solid of the aluminum material to be detected in each water washing is (5-10):1, and the unit of the liquid to solid ratio is mg/L;
preferably, the water washing of step (1) is accompanied by ultrasound.
6. The assay method of any one of claims 1-5, wherein the drying of step (1) is drying using an infrared drying lamp.
7. The analytical method of any one of claims 1 to 6, wherein the mass ratio of the tungsten-tin flux to the pure iron flux in step (2) is (1.2-1.6): 1;
preferably, the mass percent of tin in the tungsten-tin fluxing agent is 12-21%, and the balance is tungsten and inevitable impurities;
preferably, the C in the tungsten-tin fluxing agent is less than or equal to 6ppm, and the S is less than or equal to 6 ppm.
8. The assay of any one of claims 1-7, further comprising a pre-treatment step prior to step (1): and (3) sequentially crushing and screening the aluminum material to be detected, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1).
9. The analytical method according to any one of claims 1 to 8, wherein the infrared absorption method of step (2) is performed in a LECO CS844 carbon sulfur analyzer.
10. An assay method according to any one of claims 1 to 9, wherein the assay method comprises the steps of:
pretreatment: sequentially crushing and screening the aluminum material to be detected with the purity of more than or equal to 5N, and selecting the aluminum material to be detected with the granularity of 20-50 meshes to perform the step (1);
(1) sequentially carrying out acid washing, water washing and acetone washing on the aluminum material to be detected, and drying by using an infrared drying lamp to obtain a pretreated aluminum material; the pickling solution for pickling is formed by mixing hydrofluoric acid, nitric acid and deionized water according to the volume ratio of (1-2) to (6-8), wherein the concentration of the hydrofluoric acid is 35-40 wt%, and the concentration of the nitric acid is 65-70 wt%;
the number of pickling times is at least 3, the pickling time is at least 1min, the ratio of the consumption of pickling solution to the liquid-solid ratio of the aluminum material to be detected in each pickling process is (5-10):1, and the unit of the liquid-solid ratio is mg/L;
the washing times are at least 3, the washing time is at least 2min, the ratio of the consumption of deionized water to the liquid-solid ratio of the aluminum material to be detected in each washing is (5-10):1, and the unit of the liquid-solid ratio is mg/L; the water washing is accompanied by ultrasound;
(2) measuring the pretreated aluminum material obtained in the step (1) by using an infrared absorption method; the fluxing agent used by the infrared absorption method is a combination of tungsten tin fluxing agent and pure iron fluxing agent in a mass ratio of (1.2-1.6) to 1;
the mass percent of tin in the tungsten-tin fluxing agent is 12-21%, C is less than or equal to 6ppm, S is less than or equal to 6ppm, and the balance is tungsten.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011146711.1A CN112345482A (en) | 2020-10-23 | 2020-10-23 | Analysis method for carbon content in aluminum material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011146711.1A CN112345482A (en) | 2020-10-23 | 2020-10-23 | Analysis method for carbon content in aluminum material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112345482A true CN112345482A (en) | 2021-02-09 |
Family
ID=74359961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011146711.1A Pending CN112345482A (en) | 2020-10-23 | 2020-10-23 | Analysis method for carbon content in aluminum material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112345482A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113959809A (en) * | 2021-10-28 | 2022-01-21 | 宁波江丰电子材料股份有限公司 | Method for detecting oxygen content in molybdenum and molybdenum alloy |
| CN113686806B (en) * | 2021-09-24 | 2024-04-02 | 广东韶钢松山股份有限公司 | Method for detecting carbon and sulfur content in spring |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103245633A (en) * | 2013-05-16 | 2013-08-14 | 内蒙古包钢钢联股份有限公司 | Method of measuring carbon and sulfur contents in rare earth aluminum alloy through different reference material calibration infrared absorption method |
| CN104458637A (en) * | 2014-12-16 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for testing ultra-low carbon and sulphur content in plain carbon steel-low alloy steel |
| CN107153045A (en) * | 2017-06-30 | 2017-09-12 | 马鞍山钢铁股份有限公司 | A kind of method that infrared absorption determines carbon content in covering agent in Ultra-low carbon |
| CN109540830A (en) * | 2018-12-25 | 2019-03-29 | 河钢股份有限公司 | A kind of method of carbon content in measurement ferro-niobium |
| CN111304604A (en) * | 2020-03-03 | 2020-06-19 | 宁波江丰电子材料股份有限公司 | Diffusion welding method for copper target and aluminum alloy back plate and prepared copper target assembly |
| CN111501050A (en) * | 2020-04-30 | 2020-08-07 | 宁波江丰电子材料股份有限公司 | Surface treatment method of ultra-high purity aluminum |
-
2020
- 2020-10-23 CN CN202011146711.1A patent/CN112345482A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103245633A (en) * | 2013-05-16 | 2013-08-14 | 内蒙古包钢钢联股份有限公司 | Method of measuring carbon and sulfur contents in rare earth aluminum alloy through different reference material calibration infrared absorption method |
| CN104458637A (en) * | 2014-12-16 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for testing ultra-low carbon and sulphur content in plain carbon steel-low alloy steel |
| CN107153045A (en) * | 2017-06-30 | 2017-09-12 | 马鞍山钢铁股份有限公司 | A kind of method that infrared absorption determines carbon content in covering agent in Ultra-low carbon |
| CN109540830A (en) * | 2018-12-25 | 2019-03-29 | 河钢股份有限公司 | A kind of method of carbon content in measurement ferro-niobium |
| CN111304604A (en) * | 2020-03-03 | 2020-06-19 | 宁波江丰电子材料股份有限公司 | Diffusion welding method for copper target and aluminum alloy back plate and prepared copper target assembly |
| CN111501050A (en) * | 2020-04-30 | 2020-08-07 | 宁波江丰电子材料股份有限公司 | Surface treatment method of ultra-high purity aluminum |
Non-Patent Citations (1)
| Title |
|---|
| 张环月等: "高频燃烧红外吸收法测定铝钛碳中间合金中碳", 《冶金分析》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113686806B (en) * | 2021-09-24 | 2024-04-02 | 广东韶钢松山股份有限公司 | Method for detecting carbon and sulfur content in spring |
| CN113959809A (en) * | 2021-10-28 | 2022-01-21 | 宁波江丰电子材料股份有限公司 | Method for detecting oxygen content in molybdenum and molybdenum alloy |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jackson et al. | Advantages of reaction cell ICP-MS on doubly charged interferences for arsenic and selenium analysis in foods | |
| CN112345482A (en) | Analysis method for carbon content in aluminum material | |
| CN107843478A (en) | Preparation method and ultra-pure aluminum sample impurity analysis method for the ultra-pure aluminum sample of GDMS detections | |
| CN110470724A (en) | The measuring method of trace impurity in a kind of high-purity silicon dioxide | |
| CN111501050A (en) | Surface treatment method of ultra-high purity aluminum | |
| US20160320275A1 (en) | Method for determining a concentration of metal impurities contaminating a silicon product | |
| Vassileva et al. | Certification measurement of the cadmium, copper and lead contents in rice using isotope dilution inductively coupled plasma mass spectrometry | |
| Liu et al. | Fast and High Sensitive Analysis of Lead in Human Blood by Direct Sampling Hydride Generation Coupled with in situ Dielectric Barrier Discharge Trap | |
| Park et al. | A technique to minimize impurity signal from blank rhenium filaments for highly accurate TIMS measurements of uranium in ultra-trace levels | |
| CN112198184A (en) | Analysis method for detecting indium element content and distribution of high-purity aluminum target material after acid washing by EPMA | |
| CN114739926B (en) | Method for measuring residual quantity of harmful heavy metals in printing ink | |
| CN103728199B (en) | A kind of analyzing carbon-sulfure elements method in high purity copper | |
| CN116893157A (en) | Analysis method for low carbon content in ultra-high purity titanium | |
| CN111579340A (en) | Pretreatment method and oxygen content detection method for ultra-high purity aluminum/aluminum alloy sample | |
| Busheina et al. | Determination of trace elements in gallium arsenide by graphite-furnace atomic absorption spectrometry after pretreatment in gas streams | |
| CN110631874B (en) | Sample pretreatment method for determining content of silicon element in polymer and method for determining content of silicon element in polymer | |
| CN111099593B (en) | Solid reducing agent and preparation method and application thereof | |
| CN112683611A (en) | Digestion solution and method for determining element content in refined aluminum ingot for remelting | |
| CN112082834A (en) | Preparation method of quality control sample for analyzing copper content of chemical components of blister copper and anode copper | |
| CN113588584B (en) | Method for measuring oxygen content in lanthanum, cerium metal or lanthanum-cerium alloy | |
| JP4559932B2 (en) | Method for analyzing metal impurities | |
| EP1433752A1 (en) | METHOD FOR PRODUCING POTASSIUM FLUOROTANTALATE CRYSTAL BEING LOW IN OXYGEN CONTENT AND METHOD FOR PRODUCING POTASSIUM FLUORONIOBATE CRYSTAL BEING LOW IN OXYGEN CONTENT, POTASSIUM FLUOROTANTALATE CRYSTAL BEING LOW IN OXYGEN CONTENT AND POTASSIUM FLUORONIOBATE CRYSTAL BEING LOW IN OXYGEN PRODUCE | |
| Wei et al. | Adapt to the Development of Aero-engine Materials and Improve the Level of Trace Sulfur Detection | |
| CN113092550A (en) | Method for detecting chloride ion content of ferric oxide powder | |
| CN115326864A (en) | Method for measuring oxygen and nitrogen contents in lanthanum-cerium rare earth steel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |