CN104458370A - Method for preparing glow discharge mass spectrometer analysis test sample - Google Patents
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- CN104458370A CN104458370A CN201410674371.8A CN201410674371A CN104458370A CN 104458370 A CN104458370 A CN 104458370A CN 201410674371 A CN201410674371 A CN 201410674371A CN 104458370 A CN104458370 A CN 104458370A
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Abstract
The invention discloses a method for preparing a glow discharge mass spectrometer analysis test sample. The method comprises the following steps: a) putting refractory metal powder to be analyzed into a graphite mold which is internally coated with a demolding agent; b) forming the powder by using a pressure sintering method; c) milling a formed blank. By using the method disclosed by the invention, the test sample is relatively high in compactness and is clean in surface while the content of impurities in the sample is kept unchanged as much as possible, so that the accuracy and the precision of the glow discharge mass spectrum analysis result are ensured, and meanwhile the test sample prepared by using the method has the advantages of high analysis speed and high efficiency.
Description
Technical field
The present invention relates to the preparation method of a kind of glow discharge mass spectroscopy (GDMS) analytical sample.
Background technology
In the purity analysis of current a lot of high pure element or alloy, need to use glow discharge mass spectroscopy (GDMS).Glow discharge mass spectroscopy is a kind of instrument that directly can carry out impurity analysis to solid-state conductive sample, its principle is that the ionic bombardment sample surfaces that glow discharge ion source utilizes inert gas (being generally argon gas) to produce under the voltage of upper kilovolt makes it to sputter, the sample atoms that sputtering produces diffuses to further ionization in plasma, and then is collected detection by mass analyzer.Main in the world is at present the Element GD type glow discharge mass spectroscopy produced by Thermo Electron company of the U.S. at the glow discharge mass spectroscopy produced and sell, this kind of equipment can detect and nearly all element in quantitative test solid sample, comprises carbon, oxygen and nitrogen.A lot of element can be as accurate as the magnitude of more than ppb (part per billion).
For powdered sample, directly can not adopt glow discharge mass spectroscopy analysis, just can analyze after powder preparation must being become block sample.To the surface requiring to include high density and cleaning of glow discharge mass spectroscopy sample for analysis.Require that the reason of high density avoids causing the release of gas in the uneven stripping of sample and sample to produce harmful effect to analysis result because density is low; Meanwhile, also have when low density sample decomposes and the risk polluted is produced to analytical equipment.
Usually, the sample pretreatment method of GDMS comprises the step such as machinery or spark cutting, mechanical grinding, acid dissolve and cleaning, but in the process of pre-treatment, impurity is often easily introduced in the surface of sample, especially Na, Fe, Ca etc., in order to eliminate the surface contamination that sample preparation brings, the time of carrying out usually is needed to be the pre-sputtering do not waited by hour half an hour, to guarantee the Stability and veracity of collection signal.This sample preparation methods technics comparing is complicated, and the pre-sputtering time is also longer, inefficiency.In addition, for a lot of powdered sample, especially refractory metal, its body material is high-melting-point difficult to machine material, therefore, how to prepare the sample meeting and analyze and require, and do not change the impurity content of sample itself, be the problem usually run in the middle of glow discharge mass spectroscopy sample analysis process.
One of them example is ruthenium powder.High-purity ruthenium is the raw material in the widespread use of the industry such as semiconductor, hard disc of computer.Therefore, the impurity content in Water demand high-purity ruthenium powder and ruthenium block.Because ruthenium is insoluble in the characteristic of acid, make to adopt the wet-way analysis methods such as ICP-MS to become impossible.Therefore, in practical application, employing glow discharge mass spectroscopy analyzes the impurity content in ruthenium usually.For ruthenium powder, before analyzing ruthenium with glow discharge mass spectroscopy, need the ruthenium sample preparing high density, high-cleanness, high.Chinese invention patent 200610148577.2 discloses a kind of method for making of ruthenium analysis specimen, the method is in the operation of the taste utilizing glow discharge mass spectrometry device analysis ruthenium powder, the mould of the impact briquetting that material is yttrium stable zirconium oxide is used to carry out molding ruthenium powder, use in the atmosphere of reducibility gas and calcine ruthenium powder, thus preparation GDMS analyzes sample.GDMS sample rate prepared by this method is lower, affects the stability of sample analysis result.Meanwhile, in reducing atmosphere, calcine ruthenium powder, likely in calcination process, the Partial Elements existed original in powder has been reduced, thus the accuracy of impact analysis result.Therefore, how to prepare the GDMS sample of high density, surface no-pollution, the efficiency and the accuracy that improve analysis are urgent problems.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of glow discharge mass spectroscopy (GDMS) analytical sample, described sample, while the own impurity content of maintenance as far as possible, there is higher density, clean surface simultaneously, thus ensureing glow discharge mass spectrometry precision of analysis and degree of accuracy, the sample that simultaneously prepared by this preparation method also has analysis speed fast, the advantage that efficiency is high.
The object of the present invention is achieved like this:
The refractory metal powder of Water demand is positioned over inside to be scribbled in the graphite jig of release agent, uses the method for pressure sintering to powder
Carry out shaping; Turning is carried out to shaping blank.
Contribute to shaping rear material base on the one hand deviates from from mould, also prevents sample and mould on the other hand to use the reason of release agent to be
Produce chemical reaction, thus contaminated samples.
Preferably, described release agent is aluminium oxide, zirconia or boron nitride, adopts these release agents, can easily by powder-like
Product are deviate from from graphite jig.
Preferably, described pressure sintering method comprises vacuum hotpressing, discharge plasma sintering and DC heating sintering.
Preferably, described turning adopts diamond cutter, carbide-tipped tool or cubic boron nitride cutting tool, selects the reason of these cutters
Be, these cutters have higher hardness, can not only ensure the turning to sample, also can not produce residual by sample surfaces again.
Preferably, described powder is ruthenium powder.
The present invention, by the technique of pressure sintering, has prepared the analysis material base of density more than 95%, by carrying out turning surface process to analysis material base, makes the surface of analysis material base have good surface cleanliness; Meanwhile, use pressure sintering to add the preparation method of machining, any impurity be brought or be reduced to preparation process can not into, ensure that accuracy and the degree of accuracy of the result that sample is analyzed for glow discharge mass spectrometry.Therefore it is high that the analytical sample prepared has density, the features such as clean surface, thus ensure glow discharge mass spectrometry precision of analysis and degree of accuracy, and the sample that simultaneously prepared by this preparation method also has analysis speed fast, the advantage that efficiency is high.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of embodiments of the invention.
Fig. 2 is the relation of Fe, Ca, Na content and sputtering time in embodiment 1.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated, but limited the present invention never in any form, and any change done based on training centre of the present invention or improvement, all belong to protection scope of the present invention.
First, provide the powder of Water demand, such as ruthenium powder.Powder packing is scribbled in the graphite jig of release agent in inside, uses the method for pressure sintering to carry out shaping to powder; Turning is carried out to shaping blank.
Preferably, described release agent is aluminium oxide, zirconia or boron nitride.Contribute to shaping rear material base on the one hand deviates from from mould, also prevents sample and mould to produce chemical reaction on the other hand to use the reason of release agent to be, thus contaminated samples.
Described pressure sintering method comprises vacuum hotpressing, discharge plasma sintering and DC heating sintering.The advantage of pressure sintering is the density that can improve sample on the one hand, simultaneously because sintering process is in vacuum state, avoids extraneous pollution, the original impurity of powder can be kept not change simultaneously.
Preferably, described turning adopts diamond cutter, carbide-tipped tool or cubic boron nitride cutting tool, selects the reason of these cutters
Be, these cutters have higher hardness, can not only ensure the turning to sample, also can not produce residual at sample surfaces.
Preferably, described powder is ruthenium powder.
Be specifically described for the preparation method of glow discharge mass spectroscopy analysis analysis sample in the present invention below in conjunction with specific embodiment.
Ruthenium powder to be analyzed loading scribbles in the middle of the graphite jig of aluminium oxide by embodiment 1, and the internal diameter of graphite jig is 30mm, and adopt the method for vacuum hotpressing, by the pressure sintering of ruthenium powder at the temperature of 1300 DEG C, institute's applied pressure is 40MPa.Sinter rear employing Archimedes method and density has been surveyed to gained ruthenium block, 99% of ruthenium solid density can have been reached.Polycrystalline cubic boron nitride lathe tool is adopted ruthenium block to be lathed the ruthenium sample that diameter is 28mm.With acetone, ethanol and ultrapure water, ultrasonic cleaning is carried out to ruthenium sample respectively, and dry.Sample is put into ElementGD bulk sample platform, and carry out the pre-sputtering of certain hour, with Na, Fe, Ca of easily polluting for target, image data is started time basicly stable with concentration, the time of record pre-sputtering, five groups of data of collecting part typical element simultaneously, and calculate its relative standard deviation (RSD%), the repeatability of evaluation analysis result is carried out with this.Its result as shown in Table 1 and Table 2.As can be seen from Table 1 and Table 2, the pre-sputtering time of the sample prepared in the present embodiment is 10 minutes, and surface is cleaner.The RSD% of typical element content is all less than 7.5% simultaneously, has and analyzes repeatability preferably.
Embodiment 2
Being loaded by ruthenium powder to be analyzed scribbles in the middle of zirconic graphite jig, and the internal diameter of graphite jig is 30mm, and adopt the method for discharge plasma sintering, by the pressure sintering of ruthenium powder at the temperature of 1000 DEG C, institute's applied pressure is 20MPa.Sinter rear employing Archimedes method and density has been surveyed to gained ruthenium block, 95% of ruthenium solid density can have been reached.Carbide-tipped lathe tool is adopted ruthenium block to be lathed the ruthenium sample that diameter is 28mm.With acetone, ethanol and ultrapure water, ultrasonic cleaning is carried out to ruthenium sample respectively, and dry.Sample is put into Element GD bulk sample platform, and carry out the pre-sputtering of certain hour.With Na, Fe, Ca of easily polluting for target, image data is started, the time of record pre-sputtering, simultaneously five groups of data of collecting part typical element time basicly stable with its concentration, and calculate its relative standard deviation (RSD%), the repeatability of evaluation analysis result is carried out with this.Its result as shown in Table 1 and Table 2.Table 1 and table 2 can be found out, the pre-sputtering time of the sample prepared in the present embodiment is 8 minutes, and surface is cleaner.The RSD% of typical element content is all less than 8.4% simultaneously, has and analyzes repeatability preferably.
Embodiment 3
Loaded in the middle of the graphite jig scribbling boron nitride by ruthenium powder to be analyzed, the internal diameter of graphite jig is 30mm, and adopt the method for DC heating sintering, by the pressure sintering of ruthenium powder at the temperature of 1200, institute's applied pressure is 30MPa.Sinter rear employing Archimedes method and density has been surveyed to gained ruthenium block, 97% of ruthenium solid density can have been reached.Diamond bit is adopted ruthenium block to be lathed the ruthenium sample that diameter is 28mm.With acetone, ethanol and ultrapure water, ultrasonic cleaning is carried out to ruthenium sample respectively, and dry.Sample is put into Element GD bulk sample platform, and carry out the pre-sputtering of certain hour.With Na, Fe, Ca of easily polluting for target, image data is started, the time of record pre-sputtering, simultaneously five groups of data of collecting part typical element time basicly stable with its concentration, and calculate its relative standard deviation (RSD%), the repeatability of evaluation analysis result is carried out with this.Its result as shown in Table 1 and Table 2.Table 1 and table 2 can be found out, the pre-sputtering time of the sample prepared in the present embodiment is 10 minutes, and surface is cleaner.The RSD% of typical element content is all less than 7.2% simultaneously, has and analyzes repeatability preferably.
Comparative example 1
Loaded in the middle of yttrium stable zirconium oxide mould by ruthenium powder to be analyzed, the internal diameter of mould is 30mm, adopts the method for ordinary sinter, by ruthenium powder sintering at the temperature of 1000.Sinter rear employing Archimedes method and density has been surveyed to gained ruthenium block, 80% of ruthenium solid density can have been reached.With acetone, ethanol and ultrapure water, ultrasonic cleaning is carried out to ruthenium sample respectively, and dry.Sample is put into Element GD bulk sample platform, and carry out the pre-sputtering of certain hour.With Na, Fe, Ca of easily polluting for target, image data is started, the time of record pre-sputtering, simultaneously five groups of data of collecting part typical element time basicly stable with its concentration, and calculate its relative standard deviation (RSD%), the repeatability of evaluation analysis result is carried out with this.Its result as shown in Table 1 and Table 2.Table 1 and table 2 can be found out, in comparative example 1, the pre-sputtering time of the sample of preparation is 24 minutes, and sample making course may exist pollution.The maximum RSD% of typical element content is 11.8% simultaneously, and it is poor compared with comparative example that it analyzes repeatability.
Table 1 in embodiment and comparative example survey the impurity content of ruthenium powder and respective standard poor
Table 2 embodiment and comparative example pre-sputtering time and standard deviation statistics
Claims (6)
1. a preparation method for glow discharge mass spectroscopy analytical sample, is characterized in that, comprises the following steps:
A) powder of Water demand being positioned over inwall scribbles in the graphite jig of release agent;
B) method of pressure sintering is used to carry out shaping to described powder;
C) surperficial turning is carried out to shaping material base;
D) material base described in carries out cleaning-drying.
2. the method for the preparation of glow discharge mass spectroscopy analytical sample according to claim 1, is characterized in that, described release agent is aluminium oxide, zirconia or boron nitride.
3. the method for the preparation of glow discharge mass spectroscopy analytical sample according to claim 1, is characterized in that, described pressure sintering method comprises vacuum hotpressing, discharge plasma sintering and DC heating sintering.
4. the method for the preparation of glow discharge mass spectroscopy analytical sample according to claim 1, is characterized in that, described turning adopts carbide-tipped tool, diamond cutter or cubic boron nitride cutting tool.
5. the method for the preparation of glow discharge mass spectroscopy analytical sample according to claim 1, is characterized in that, described powder is ruthenium powder.
6. a preparation method for glow discharge mass spectroscopy analytical sample ruthenium powder, is characterized in that, comprise the following steps:
Loaded in the middle of the graphite jig scribbling aluminium oxide by ruthenium powder to be analyzed, the internal diameter of graphite jig is 30mm, and adopt the method for vacuum hotpressing, by the pressure sintering of ruthenium powder at the temperature of 1300 DEG C, institute's applied pressure is 40MPa;
Sinter rear employing Archimedes method and density has been surveyed to gained ruthenium block, 99% of ruthenium solid density can have been reached;
Polycrystalline cubic boron nitride lathe tool is adopted ruthenium block to be lathed the ruthenium sample that diameter is 28mm;
With acetone, ethanol and ultrapure water, ultrasonic cleaning is carried out to ruthenium sample respectively, and dry;
Sample is put into Element GD bulk sample platform, and carry out the pre-sputtering of certain hour, with Na, Fe, Ca of easily polluting for target, image data is started time basicly stable with concentration, the time of record pre-sputtering, five groups of data of collecting part typical element simultaneously, and calculate its relative standard deviation (RSD%), the repeatability of evaluation analysis result is carried out with this.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105628785A (en) * | 2015-12-25 | 2016-06-01 | 中国计量科学研究院 | High-purity copper correction sample for glow discharge mass spectrometer and preparation method of high-purity copper correction sample |
| CN106198712A (en) * | 2016-06-24 | 2016-12-07 | 锦州市国家光伏材料质量监督检验中心 | The method of trace impurity content in a kind of glow discharge spectrometry detection metal |
| CN108680411A (en) * | 2018-05-31 | 2018-10-19 | 宁波江丰电子材料股份有限公司 | High purity tungsten sample and preparation method thereof for GDMS detections |
| CN108918226A (en) * | 2018-07-23 | 2018-11-30 | 江苏隆达超合金航材有限公司 | A kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens |
| CN110186997A (en) * | 2019-06-14 | 2019-08-30 | 新疆众和股份有限公司 | The method that glow discharge spectrometry detects impurity content in aluminium hydroxide |
| CN111487097A (en) * | 2020-03-24 | 2020-08-04 | 上海材料研究所 | Method for preparing high-performance blocky standard sample blank by using powder as raw material |
| CN113433208A (en) * | 2021-05-18 | 2021-09-24 | 紫金矿业集团黄金冶炼有限公司 | Preparation method for detecting 6N copper sample by GDMS (gas chromatography mass spectrometry) and low-S test method |
| CN114112602A (en) * | 2021-12-20 | 2022-03-01 | 昆明理工大学 | Pretreatment method for detecting small amount of fragile sample for ELEMENT GD glow discharge mass spectrum detection |
| CN117451465A (en) * | 2023-12-26 | 2024-01-26 | 浙江大学海南研究院 | Preparation method of standard substance, standard substance and application method of standard substance |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020018921A1 (en) * | 2000-04-18 | 2002-02-14 | Ngk Insulators, Ltd. | Halogen gas plasma-resistive members and method for producing the same, laminates, and corrosion-resistant members |
| CN101046433A (en) * | 2006-03-31 | 2007-10-03 | 日矿金属株式会社 | Method of manufacturing analysis specimen |
| CN102605332A (en) * | 2012-03-25 | 2012-07-25 | 昆明贵金属研究所 | Ru sputtering target with high purity and preparation method thereof |
| CN102922231A (en) * | 2012-10-25 | 2013-02-13 | 昆明贵金属研究所 | Method for machining ruthenium and ruthenium alloy target |
-
2014
- 2014-11-23 CN CN201410674371.8A patent/CN104458370A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020018921A1 (en) * | 2000-04-18 | 2002-02-14 | Ngk Insulators, Ltd. | Halogen gas plasma-resistive members and method for producing the same, laminates, and corrosion-resistant members |
| CN101046433A (en) * | 2006-03-31 | 2007-10-03 | 日矿金属株式会社 | Method of manufacturing analysis specimen |
| CN102605332A (en) * | 2012-03-25 | 2012-07-25 | 昆明贵金属研究所 | Ru sputtering target with high purity and preparation method thereof |
| CN102922231A (en) * | 2012-10-25 | 2013-02-13 | 昆明贵金属研究所 | Method for machining ruthenium and ruthenium alloy target |
Non-Patent Citations (2)
| Title |
|---|
| 苏永选 等: "辉光放电质谱研究与应用新进展", 《分析测试学报》 * |
| 荣百炼 等: "辉光放电质谱法测定高纯锑中的痕量杂质元素", 《质谱学报》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105628785A (en) * | 2015-12-25 | 2016-06-01 | 中国计量科学研究院 | High-purity copper correction sample for glow discharge mass spectrometer and preparation method of high-purity copper correction sample |
| CN106198712A (en) * | 2016-06-24 | 2016-12-07 | 锦州市国家光伏材料质量监督检验中心 | The method of trace impurity content in a kind of glow discharge spectrometry detection metal |
| CN108680411A (en) * | 2018-05-31 | 2018-10-19 | 宁波江丰电子材料股份有限公司 | High purity tungsten sample and preparation method thereof for GDMS detections |
| CN108918226A (en) * | 2018-07-23 | 2018-11-30 | 江苏隆达超合金航材有限公司 | A kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens |
| CN108918226B (en) * | 2018-07-23 | 2020-07-24 | 江苏隆达超合金航材有限公司 | Preparation method of titanium sponge and titanium crystal grain sample for GDMS (gas chromatography mass spectrometry) detection |
| CN110186997A (en) * | 2019-06-14 | 2019-08-30 | 新疆众和股份有限公司 | The method that glow discharge spectrometry detects impurity content in aluminium hydroxide |
| CN111487097A (en) * | 2020-03-24 | 2020-08-04 | 上海材料研究所 | Method for preparing high-performance blocky standard sample blank by using powder as raw material |
| CN113433208A (en) * | 2021-05-18 | 2021-09-24 | 紫金矿业集团黄金冶炼有限公司 | Preparation method for detecting 6N copper sample by GDMS (gas chromatography mass spectrometry) and low-S test method |
| CN114112602A (en) * | 2021-12-20 | 2022-03-01 | 昆明理工大学 | Pretreatment method for detecting small amount of fragile sample for ELEMENT GD glow discharge mass spectrum detection |
| CN114112602B (en) * | 2021-12-20 | 2023-12-22 | 昆明理工大学 | Pre-detection treatment method for small amount of fragile sample for ELEMENT GD glow discharge mass spectrum detection |
| CN117451465A (en) * | 2023-12-26 | 2024-01-26 | 浙江大学海南研究院 | Preparation method of standard substance, standard substance and application method of standard substance |
| CN117451465B (en) * | 2023-12-26 | 2024-04-05 | 浙江大学海南研究院 | Preparation method of standard substance, standard substance and application method of standard substance |
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