CN103175777A - Analytical method for oxygen content in metal powder - Google Patents
Analytical method for oxygen content in metal powder Download PDFInfo
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- CN103175777A CN103175777A CN2012101885395A CN201210188539A CN103175777A CN 103175777 A CN103175777 A CN 103175777A CN 2012101885395 A CN2012101885395 A CN 2012101885395A CN 201210188539 A CN201210188539 A CN 201210188539A CN 103175777 A CN103175777 A CN 103175777A
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Abstract
The invention belongs to a gas analytical technology in the field of analytical chemistry, and relates to an improvement of an analytical method for oxygen content in metal powder. The improvement comprises the steps of putting the to-be-detected metal powder into a high-purity nickel pocket or a nickel foil, packaging and compacting the to-be-detected metal powder, and expelling air in the pocket; putting the nickel pocket or the nickel foil into a graphite crucible in a pulse heating furnace, and opening a power gas to ascend a lower electrode, thus enabling the graphite crucible to be contacted with a fixed upper electrode; electrifying to melt the to-be-detected powder in the nickel pocket or the nickel foil at high temperature, and conveying the gas in the pulse heating furnace into a dust filter under the driving of a helium gas flow, and filtering to remove dust; oxidizing carbon monoxide in the gas subjected to dust removal by filtering into carbon dioxide via a catalysis furnace; and conveying the gas passing through the catalysis furnace into an infrared detection pond via a flow controller, so as to detect the content of oxygen. The technical scheme disclosed by the invention is simple in device, simple, convenient and practical to operate, and capable of avoiding the problem of the influence on the analytical precision of an instrument or damages on the instrument caused by the outward sputtering and attachment of the powder in the analytical channel of the instrument.
Description
Technical field
The invention belongs to analytical chemistry field gas analysis technology, relate to the improvement of the analytical approach of oxygen content in metal powder.
Background technology
The silver-bearing copper powder is in certain aeromotor manufacturing, the parts such as dish, axle to be carried out the coating material of plasma spraying, according to the plasma spray coating process requirement, oxygen content in this dusty material is less than 0.12%, when originally measuring the method for oxygen content in metal powder in laboratory condition, adopt oxygen-nitrogen analyzer, directly be positioned over metal powder in graphite crucible, when the metal powder high-temperature fusion, can produce splash, adhere in the instrumental analysis passage, affect the instrumental analysis precision or damage instrument, thereby can't carry out the analysis of oxygen content in metal powder.
Summary of the invention
The objective of the invention is: propose a kind of analytical approach of measuring oxygen content in metal powder with nickel capsule parcel powdered sample, avoid the outer spatter of powder in the instrumental analysis passage, affect the instrumental analysis precision or damage instrument.
Technical scheme of the present invention is: the analytical approach of oxygen content in a kind of metal powder, utilize oxygen-nitrogen analyzer, and it is characterized in that, comprise the steps:
The first, metal powder to be measured is put into high purity nickel capsule or nickel foil, with its parcel and compacting, catch up with except the air in parcel;
The second, with the above-mentioned nickel capsule of metal powder to be measured or the graphite crucible of the pulse heating furnace that nickel foil is put into oxygen-nitrogen analyzer of having wrapped up, open power gas and make bottom electrode increase, make graphite crucible contact with fixing top electrode;
The 3rd, energising, make powder to be measured melting in nickel capsule or nickel foil, under helium flow drove, the gas in pulse heating furnace (carbon monoxide or the carbon dioxide that form after the oxygen that discharges in melting process and graphite reaction) entered into the dust filter unit dust removal by filtration;
The 4th, the Oxidation of Carbon Monoxide of inciting somebody to action wherein by catalyst furnace through the gas of above-mentioned dust removal by filtration becomes carbon dioxide;
The 5th, above-mentioned gas by catalyst furnace enters into infrared detection pond through flow controller, detects the content of oxygen.
Advantage of the present invention is: the technical solution of the present invention device is simple, easy to operation, avoid the outer spatter of powder in the instrumental analysis passage, affected the problem of instrumental analysis precision or damage instrument, can not analyze the situation of oxygen content in For Metal Powder Sample at present thereby solved.
Description of drawings
Fig. 1: oxygen-nitrogen analyzer structural representation
Fig. 2: nickel capsule structural representation
1-helium gas source, 2-pressure switch, 3-filtrator, 3a-alkali asbestos, the anhydrous magnesium perchlorate of 3b-, 4-flow stabilizing valve, 5-pulse heating furnace, 5a-top electrode, 5b-bottom electrode, 5c-graphite crucible, 6-dust filter unit, 7-catalyst furnace, 8-flow controller, 9-infrared detection pond, 10-power gas source
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further details.Referring to Fig. 1, it is characterized in that, oxygen-nitrogen analyzer is comprised of helium gas source 1, pressure switch 2, filtrator 3, flow stabilizing valve 4, pulse heating furnace 5, dust filter unit 6, catalyst furnace 7, flow controller 8, infrared detection pond 9, power gas 10; Be connected with the air intake opening of alkali asbestos, anhydrous magnesium perchlorate's filtrator 3 by regulating pressure switch 2, flow stabilizing valve 4 is connected with the air intake opening of being connected with pulse heating furnace in the gas outlet of alkali asbestos, anhydrous magnesium perchlorate's filtrator 3 respectively; Analytic sample is in pulse heating furnace 5 after high-temperature fusion, the CO gas that discharges enters into dust filter unit 6 dust removals by filtration with helium, through catalyst furnace 7, Oxidation of Carbon Monoxide is become carbon dioxide, regulate a certain amount of air-flow by flow controller 8 at last and make carbon dioxide enter into the content that infrared detection pond 9 detects oxygen.
Embodiment 1, the analytical approach of oxygen content in the silver-bearing copper powder.
Analytical procedure is as follows:
The first, the silver-bearing copper powdered sample that takes about 0.5g is put into high purity nickel capsule parcel and compacting, drives air away, and the testing sample after parcel and compacting is dropped in graphite crucible, opens power gas and makes bottom electrode increase to contact by graphite crucible with fixing top electrode.
The second, energising, setting degassed power is 6000w, analyzes power 5500w.Sample is high-temperature fusion in pulse heating furnace, the CO gas that discharges enters into the dust filter unit dust removal by filtration with helium, through catalyst furnace, it is oxidized to carbon dioxide again, enters into by flow controller the content that infrared detection pond detects oxygen at last.
The 3rd, open pulse heating furnace, bottom electrode is descended, take out graphite crucible.
Embodiment 2, the analytical approach of oxygen content in nichrome powder.
Analytical procedure is as follows:
First, the nichrome powder sample that takes about 0.3g is put into high purity nickel capsule parcel and compacting, drive air away, the testing sample after parcel and compacting is dropped in graphite crucible, open power gas and make bottom electrode increase to contact by graphite crucible with fixing top electrode.
The second, energising, setting degassed power is 5500w, analyzes power 5000w.Sample is high-temperature fusion in pulse heating furnace, the CO gas that discharges enters into the dust filter unit dust removal by filtration with helium, through catalyst furnace, it is oxidized to carbon dioxide again, enters into by flow controller the content that infrared detection pond detects oxygen at last.
The 4th, open pulse heating furnace, bottom electrode is descended, take out graphite crucible.
Analytical procedure is as follows:
First, the nickel alclad alloy powder sample that takes about 0.3g is with also compacting of parcel in high-purity nickel foil, drive air away, the testing sample after parcel and compacting is dropped in graphite crucible, open power gas and make bottom electrode increase to contact by graphite crucible with fixing top electrode.
The second, energising, setting degassed power is 6500w, analyzes power 6000w.Sample is high-temperature fusion in pulse heating furnace, the CO gas that discharges enters into the dust filter unit dust removal by filtration with helium, through catalyst furnace, it is oxidized to carbon dioxide again, enters into by flow controller the content that infrared detection pond detects oxygen at last.
The 5th, open pulse heating furnace, bottom electrode is descended, take out graphite crucible.
Claims (1)
1. the analytical approach of oxygen content in a metal powder, utilize oxygen-nitrogen analyzer, it is characterized in that, comprises the steps:
The first, metal powder to be measured is put into high purity nickel capsule or nickel foil, with its parcel and compacting, catch up with except the air in parcel;
The second, with the above-mentioned nickel capsule of metal powder to be measured or the graphite crucible of the pulse heating furnace that nickel foil is put into oxygen-nitrogen analyzer of having wrapped up, open power gas and make bottom electrode increase, make graphite crucible contact with fixing top electrode;
The 3rd, energising, make powder to be measured melting in nickel capsule or nickel foil, under helium flow drove, the gas in pulse heating furnace (carbon monoxide or the carbon dioxide that form after the oxygen that discharges in melting process and graphite reaction) entered into the dust filter unit dust removal by filtration;
The 4th, the Oxidation of Carbon Monoxide of inciting somebody to action wherein by catalyst furnace through the gas of above-mentioned dust removal by filtration becomes carbon dioxide;
The 5th, above-mentioned gas by catalyst furnace enters into infrared detection pond through flow controller, detects the content of oxygen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101885395A CN103175777A (en) | 2011-12-20 | 2012-06-08 | Analytical method for oxygen content in metal powder |
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| CN201110431531.2 | 2011-12-20 | ||
| CN201110431531 | 2011-12-20 | ||
| CN2012101885395A CN103175777A (en) | 2011-12-20 | 2012-06-08 | Analytical method for oxygen content in metal powder |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103529187A (en) * | 2013-10-17 | 2014-01-22 | 浙江衢州永丰金属制品有限公司 | Method for measuring oxygen content in iron powder |
| CN104034664A (en) * | 2014-05-30 | 2014-09-10 | 中国船舶重工集团公司第七二五研究所 | Method for determining oxygen content of flux-cored wire powder and soldering flux |
| CN105136661A (en) * | 2015-09-18 | 2015-12-09 | 苏州萨伯工业设计有限公司 | Oxygen and nitrogen analyzer |
| CN106370497A (en) * | 2016-11-07 | 2017-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Sample preparation method for assaying oxygen content of vanadium-aluminum alloy |
| CN107064045A (en) * | 2016-12-12 | 2017-08-18 | 中核北方核燃料元件有限公司 | The assay method of oxygen content in a kind of composite material of silicon carbide |
| CN107941738A (en) * | 2017-12-19 | 2018-04-20 | 武汉钢铁有限公司 | The method of inspection of nitrogen content in a kind of variety steel magnesium oxide coating |
| CN111089947A (en) * | 2019-11-19 | 2020-05-01 | 江苏博迁新材料股份有限公司 | Device and method for detecting high oxygen content in metal powder |
| CN111089874A (en) * | 2018-10-24 | 2020-05-01 | 宜都东阳光化成箔有限公司 | Method for detecting surface oxidation degree of aluminum powder |
| CN112098622A (en) * | 2020-08-21 | 2020-12-18 | 宁波广新纳米材料有限公司 | Device and method for detecting oxygen content of extremely-oxidizable metal powder |
| CN113985000A (en) * | 2021-10-15 | 2022-01-28 | 中国航发北京航空材料研究院 | Method for measuring content of oxygen and nitrogen elements in high-temperature alloy powder for additive manufacturing |
| CN114199641A (en) * | 2021-10-21 | 2022-03-18 | 深圳市深汕特别合作区万泽精密科技有限公司 | Method for measuring oxygen content in nickel-based superalloy powder |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103529187A (en) * | 2013-10-17 | 2014-01-22 | 浙江衢州永丰金属制品有限公司 | Method for measuring oxygen content in iron powder |
| CN103529187B (en) * | 2013-10-17 | 2015-08-05 | 浙江衢州永丰金属制品有限公司 | The assay method of oxygen content in a kind of iron powder |
| CN104034664A (en) * | 2014-05-30 | 2014-09-10 | 中国船舶重工集团公司第七二五研究所 | Method for determining oxygen content of flux-cored wire powder and soldering flux |
| CN105136661A (en) * | 2015-09-18 | 2015-12-09 | 苏州萨伯工业设计有限公司 | Oxygen and nitrogen analyzer |
| CN106370497A (en) * | 2016-11-07 | 2017-02-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Sample preparation method for assaying oxygen content of vanadium-aluminum alloy |
| CN107064045A (en) * | 2016-12-12 | 2017-08-18 | 中核北方核燃料元件有限公司 | The assay method of oxygen content in a kind of composite material of silicon carbide |
| CN107941738A (en) * | 2017-12-19 | 2018-04-20 | 武汉钢铁有限公司 | The method of inspection of nitrogen content in a kind of variety steel magnesium oxide coating |
| CN111089874A (en) * | 2018-10-24 | 2020-05-01 | 宜都东阳光化成箔有限公司 | Method for detecting surface oxidation degree of aluminum powder |
| CN111089947A (en) * | 2019-11-19 | 2020-05-01 | 江苏博迁新材料股份有限公司 | Device and method for detecting high oxygen content in metal powder |
| CN112098622A (en) * | 2020-08-21 | 2020-12-18 | 宁波广新纳米材料有限公司 | Device and method for detecting oxygen content of extremely-oxidizable metal powder |
| CN113985000A (en) * | 2021-10-15 | 2022-01-28 | 中国航发北京航空材料研究院 | Method for measuring content of oxygen and nitrogen elements in high-temperature alloy powder for additive manufacturing |
| CN114199641A (en) * | 2021-10-21 | 2022-03-18 | 深圳市深汕特别合作区万泽精密科技有限公司 | Method for measuring oxygen content in nickel-based superalloy powder |
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Application publication date: 20130626 |