CN106198588A - The detection method of objectionable impurities in a kind of transformator copper conductor - Google Patents

The detection method of objectionable impurities in a kind of transformator copper conductor Download PDF

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Publication number
CN106198588A
CN106198588A CN201610677322.9A CN201610677322A CN106198588A CN 106198588 A CN106198588 A CN 106198588A CN 201610677322 A CN201610677322 A CN 201610677322A CN 106198588 A CN106198588 A CN 106198588A
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testing sample
objectionable impurities
copper conductor
conical flask
vacuum
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CN201610677322.9A
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Inventor
何潇
郭新良
夏桓桓
何运华
杨雪滢
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Electric Power Research Institute of Yunnan Power System Ltd
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Electric Power Research Institute of Yunnan Power System Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2206Combination of two or more measurements, at least one measurement being that of secondary emission, e.g. combination of secondary electron [SE] measurement and back-scattered electron [BSE] measurement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202Preparing specimens therefor

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The embodiment of the invention discloses the detection method of objectionable impurities in a kind of transformator wire, including: tight has the testing sample of insulating paper be placed in vacuum tank, is dried 12 72 hours at a temperature of 60 ° 120 °, is cooled to 20 ° 40 °;Immerse and deaerated except in the new transformer oil of water 12 48 hours;In conical flask, add insulating oil by quality and surface area ratio 1 50, insulating oil adds the benzyl disulfide of 10 10000ppm;It is placed in vacuum nitrogen case, seals conical flask;Conical flask is placed in 80 ° 240 °, heat ageing 10 1000 hours in the vacuum ageing oven of 0.01 1MPa;Testing sample after heat ageing is detected kind and the content determining objectionable impurities.The present invention is by studying kind and the content of objectionable impurities in transformator copper conductor, for the support of the preventing and treating offer experimental data of transformer oil sulfur corrosion phenomenon.

Description

The detection method of objectionable impurities in a kind of transformator copper conductor
Technical field
The present invention relates to materials science field, particularly relate to the inspection of objectionable impurities in a kind of transformator copper conductor Survey method.
Background technology
Transformator is the core of energy conversion in electric energy transmission and delivery process, is most important in electric power netting safe running and One of crucial equipment.The major accident of transformator not only causes the damage of self, also can interrupt supply of electric power, cause to society Huge economic loss.Wherein, the problem that the coil of converting equipment and paper oil insulation material are corroded by active sulfur compound is drawn Play more and more international person skilled and the concern of researcher.
In prior art, for the etching problem to transformator wire of the active sulfur compound in insulating oil, from insulation In oil, the source of active sulfur, harm, coherent detection standard, braking measure etc. are all studied.Such as, the most relatively Being interpolation passivator in insulating oil for generally acknowledged method, passivator is phenylpropyl alcohol triazole and derivant thereof.Phenylpropyl alcohol triazole and The hetero atoms such as N, O, the S in its derivative molecular contain lone pair electrons, it is easy to and the d track combination formation coordinate bond of metal, or It is that metal provides electronics to form back coordination key to hetero atom, thus forms protecting film in metal surface, stop transformator with leading The oxidation of line and with the contacting of active sulfur in insulating oil.
But, passivator is the most gradually consumed, the protective effect of the protecting film formed on transformator wire Can gradually weaken, and in the case of transformator is by wire hot-spot or shelf depreciation, inactive sulfur changes to active sulfur, Accelerate the corrosion rate of active sulfur.Meanwhile, the sulfur product that some objectionable impurities in transformator wire and sulfur generate adds The carrying out of speed corrosion.
Summary of the invention
The embodiment of the present invention provides the detection method of objectionable impurities in a kind of transformator copper conductor, existing to solve The problem of the carrying out of the sulfur product accelerated corrosion that some objectionable impurities in transformator wire in technology generates with sulfur.
In order to solve above-mentioned technical problem, the embodiment of the invention discloses following technical scheme:
The invention discloses the detection method of objectionable impurities in a kind of transformator copper conductor, including:
The testing sample that tight has insulating paper is placed in vacuum tank, and to vacuum tank at a temperature of 60 °-120 ° After interior testing sample is dried 12-72 hour, it is cooled to 20 °-40 °;
Testing sample after cooling is immersed and has deaerated except in the new transformer oil of water 12-48 hour;
It is that 1-50 adds in conical flask in insulating oil, and insulating oil and is added with concentration and is by quality and surface area ratio The benzyl disulfide of 10-10000ppm;
Testing sample after immersion oil is loaded in described conical flask, is placed in vacuum nitrogen case, vacuum nitrogen case is entered After row evacuation nitrogen charging, seal described conical flask;
Conical flask after sealing is placed in the vacuum ageing oven of 80 °-240 °, and the vacuum at vacuum ageing oven is Heat ageing 10-1000 hour under 0.01-1MPa;
Utilize scanning electron microscope/energy disperse spectroscopy that the testing sample after heat ageing is detected;
Kind and the content of objectionable impurities is determined according to testing result.
Preferably, utilize scanning electron microscope/energy disperse spectroscopy that the sample after heat ageing is detected, including:
Utilize scanning electron microscope that testing sample surface microscopic topographic is detected, determine the position of etch pit;
Utilize the X-ray energy spectrum of energy disperse spectroscopy capture etch pit interior element;
X-ray energy spectrum analytic process is used to determine etch pit interior element kind and content.
Preferably, the described testing sample by after immersion oil loads in described conical flask, including:
Testing sample after immersion oil is inserted in described conical flask, and keeps described testing sample to lie against described conical flask Bottle at the bottom of in.
Preferably, described new transformer oil is the change not containing active sulfur compound and sulfur content less than or equal to 1000ppm Force feed.
Preferably, stating testing sample is transformator copper conductor, and the shape of described testing sample is uniform.
Preferably, the concentration of described benzyl disulfide is 200-10000ppm.
Preferably, described thermal aging time is 50-1000 hour.
Preferably, the temperature in described vacuum ageing oven is set to 120 °-200 °.
From above technical scheme, the detection of a kind of transformator copper conductor objectionable impurities that the embodiment of the present invention provides Method, by controlling the conditions such as the temperature of vacuum, copper conductor placement location, accelerated ageing, it is achieved the acceleration heat of copper conductor is old Change.Utilize scanning electron microscope/energy disperse spectroscopy that copper conductor surface microscopic appearance and etch pit interior element are formed situation to see Examine and calculate, so that it is determined that the kind of objectionable impurities and content in copper conductor, and then be the preventing and treating of transformer oil stream corrosion phenomenon Offer experimental data is supported.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, for those of ordinary skill in the art Speech, on the premise of not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
In a kind of transformator copper conductor that Fig. 1 provides for the embodiment of the present invention, the flow process of the detection method of objectionable impurities is shown It is intended to.
Detailed description of the invention
The embodiment of the present invention provides the detection method of objectionable impurities in a kind of transformator copper conductor, in order to make this technology lead The personnel in territory are more fully understood that the technical scheme in the present invention, below in conjunction with the accompanying drawing in the embodiment of the present invention, to the present invention Technical scheme in embodiment is clearly and completely described, it is clear that described embodiment is only that a part of the present invention is real Execute example rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creation The every other embodiment obtained under property work premise, all should belong to the scope of protection of the invention.
For the technical scheme making those skilled in the art be more fully understood that in the embodiment of the present invention, and make the present invention real Execute the above-mentioned purpose of example, feature and advantage can become apparent from understandable, below in conjunction with the accompanying drawings to technical side in the embodiment of the present invention Case is described in further detail.
Transformator copper conductor is a kind of high-purity red copper, and the impurity of red copper itself is more, but content is relatively low.Existing skill In art, coil and paper oil insulation material for converting equipment are studied by active sulfur compound, are primarily intended to insulating oil Research, the present invention is mainly to dopant species and determination study in transformator copper conductor.
According to metal active sequence list, the activity of partial impurities is far above copper, such as: Na, Mg, Al, Zn etc., same Under sample corrosive environment, these activity high impurity corrode prior to copper, and formed sulfur product be deposited on insulating paper or Dispersion is suspended in insulating oil;Equally, activity is less than the impurity of copper, under same corrosive environment, forms galvanic element with copper, makes bucket Corrosion is accelerated, formation cuprous sulfide in Oil-Paper Insulation, thus initiating failure.So, select suitable method, detect copper In wire, dopant species and impurity carry out oil sulfur corrosion degree to transformator, and transformator is carried out effective risk assessment and operation State estimation has great importance.
See Fig. 1, for the detection method flow process of objectionable impurities in a kind of transformer copper wire that the embodiment of the present invention provides Schematic diagram.
Step S100, has the testing sample of insulating paper to be placed in vacuum tank by tight, and the temperature of 60 °-120 ° Under the testing sample in vacuum tank is dried 12-72 hour after, be cooled to 20 °-40 °.
Transformator copper conductor utilization cutting equipment is cut into the uniform sample of some shapes, after closely wrapping insulating paper It is placed in vacuum tank.At a temperature of 60 °-120 °, testing sample is dried process, is dried 12-72 hour, at vacuum tank Inside be dried is to get rid of the corrosion to testing sample of oxygen and moisture.
Step S200, immerses the testing sample after cooling and has deaerated except in the new transformer oil of water 12-48 hour.
Before testing sample enters in new transformer oil, new transformer oil needs first to deaerate except water, gets rid of moisture and oxygen pair The corrosion of testing sample, does not contains active sulfur compound in new transformer oil, total sulfur content is less than or equal to 1000ppm, uses New transformer oil, also for the caustic got rid of in the transformer oil corrosion to testing sample.
Step S300, is that 1-50 adds interpolation in insulating oil, and insulating oil in conical flask by quality and surface area ratio The benzyl disulfide having concentration to be 10-10000ppm.
In conical flask, add insulating oil with quality with the surface area ratio ratio as 1-50, then add in insulating oil Concentration is two benzyl group two sulfur of 10-10000ppm, and wherein two benzyl group two sulfur are active sulfur.Wherein quality with surface area ratio is Relation according to power equipment copper conductor with oil determines, and owing to the contact area of copper conductor is relatively big on the impact of corrosion, So calculating according to surface area.Further, the concentration of benzyl disulfide can be controlled between 200-10000ppm.
Step S400, loads the testing sample after immersion oil in described conical flask, is placed in vacuum nitrogen case, to vacuum After nitrogen charging case carries out evacuation nitrogen charging, seal described conical flask.
Testing sample after immersion oil being loaded taper bottle-type and carries out corrosion reaction, before accelerated corrosion, needing first will cone Shape bottle seals, and gets rid of the oxygen corrosion to copper conductor, when sealing conical flask, conical flask is placed in vacuum nitrogen case, Vacuum nitrogen case is carried out after evacuation nitrogen charging again, in sealing, the nitrogen charging environment lower seal conical flask of vacuum nitrogen case.
Testing sample is put at the bottom of the bottle of conical flask, and keeps flat at the bottom of the bottle of conical flask.Lie against at the bottom of conical flask bottle In, due to the differential concentration corrosion existed at the bottom of bottle, the corrosion of copper conductor can be accelerated.
Step S500, the conical flask after sealing is placed in the vacuum ageing oven of 80 °-240 °, true at vacuum ageing oven Reciprocal of duty cycle is heat ageing 10-1000 hour under 0.10-1MPa.
Testing sample starts to be corroded 80 ° when, thus the temperature of vacuum ageing oven be adjusted to 80 °-240 ° it Between, vacuum degree control is at 0.01-1MPa, and ageing time controls at 10-1000 hour, within 10 hours, be corrosion occur minimum time Between, can be according to etching condition Comprehensive Control ageing times such as the temperature in caustic concentration, vacuum tank in process of the test.Enter one Step, thermal aging time can be controlled between 50-1000 hour, temperature in Vacuum Heat ageing oven control again 120 °-200 ° it Between.
Step S600, utilizes scanning electron microscope energy disperse spectroscopy to detect the testing sample after heat ageing.
Step S700, determines kind and the content of objectionable impurities according to testing result.
After the corrosion and ageing process of step S100-S500, the objectionable impurities in testing sample is corroded, and corrosion occurs Hole, utilizes scanning electron microscope energy disperse spectroscopy to detect the testing sample after heat ageing, and determines have according to testing result The kind of evil impurity and content.
When utilizing scanning electron microscope/energy disperse spectroscopy that testing sample is detected, first with scanning electron microscopy The surface microscopic topographic of testing sample is detected by mirror, determines the position of etch pit, because objectionable impurities can shape after being corroded Become etch pit.
Then, according to the characteristic X-ray of different elements, there is this feature of different energy, utilize energy disperse spectroscopy to obtain corrosion X-ray in hole, uses X-ray energy spectrum analytic process to determine etch pit interior element kind and content.
According to said method, it is provided that below embodiment:
Copper conductor utilizes linear cutting equipment cut into the uniform sample of some shapes, insulating paper on tight, is placed in In vacuum tank, be dried 48 hours at 90 DEG C, after be cooled to 40 DEG C, immerse and deaerated the new transformer oil except water and kept 12 little Time;
Adding two benzyl group two sulfur in insulating oil, concentration is 200ppm, and presses 1g oil: 0.5cm2The ratio of copper is to conical flask Middle interpolation insulating oil, loads the copper conductor sample after immersion oil in conical flask simultaneously, at the bottom of keeping copper bar to lie in bottle, and immerses absolutely Edge oil, after conical flask is placed in vacuum nitrogen case, evacuation and under vacuum state nitrogen charging to after a normal atmosphere Airtight, be full of nitrogen in the environment of seal;
By above-mentioned copper conductor sample as in 150 DEG C of vacuum ageing ovens, control vacuum 0.01 and carry out thermal aging test, heat Ageing time is 72 hours, and sampling measures;
There is obvious corrosion phenomenon on the testing sample surface obtained by said process, then utilizes scanning electron microscopy Copper conductor surface microscopic topographic and etch pit interior element kind are detected by mirror/energy disperse spectroscopy with content, observe etch pit size And etch pit interior element composition situation.
Obtaining cheating interior element by X-ray energy spectrum analytic process is Cu, Al, and etch pit diameter is the biggest, the Al element in hole Content is the most, and the objectionable impurities thus obtaining copper conductor is Al element.
As seen from the above-described embodiment, the detection of objectionable impurities in a kind of transformator copper conductor that the embodiment of the present invention provides Method, prepares effectively to simulate the use environment of transformator copper conductor, and realizes testing sample in vacuum ageing oven Rapid Thermal is aging, effective discharge oxygen and the moisture corrosion to copper conductor in Heat Ageing, leads for research transformer copper In line, kind and the content of objectionable impurities provide effective corrosivity copper conductor.
After obtaining the testing sample being corroded, X-ray energy spectrum analytic process is used to determine kind and the content of objectionable impurities, Preventing and treating for transformer oil sulfur corrosion phenomenon provides the support of experimental data, and utilizes experimental data to carry out transformator effectively Risk assessment and running status assessment.
It should be noted that in this article, term " includes ", " comprising " or its any other variant are intended to non-row Comprising of his property, so that include that the process of a series of key element, method, article or equipment not only include those key elements, and And also include other key elements being not expressly set out, or also include intrinsic for this process, method, article or equipment Key element.In the case of there is no more restriction, statement " including ... " key element limited, it is not excluded that including State and the process of key element, method, article or equipment there is also other identical element.
The above is only the detailed description of the invention of the present invention, makes to skilled artisans appreciate that or realize this Bright.Multiple amendment to these embodiments will be apparent to one skilled in the art, as defined herein General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one The widest scope caused.

Claims (8)

1. the detection method of objectionable impurities in a transformator copper conductor, it is characterised in that including:
The testing sample that tight has insulating paper is placed in vacuum tank, and in vacuum tank at a temperature of 60 °-120 ° After testing sample is dried 12-72 hour, it is cooled to 20 °-40 °;
Testing sample after cooling is immersed and has deaerated except in the new transformer oil of water 12-48 hour;
It is that 1-50 adds in conical flask in insulating oil, and insulating oil that to be added with concentration be 10-by quality and surface area ratio The benzyl disulfide of 10000ppm;
Testing sample after immersion oil is loaded in described conical flask, is placed in vacuum nitrogen case, vacuum nitrogen case is taken out After vacuum nitrogen charging, seal described conical flask;
Conical flask after sealing is placed in the vacuum ageing oven of 80 °-240 °, and the vacuum at vacuum ageing oven is 0.01- Heat ageing 10-1000 hour under 1MPa;
Utilize scanning electron microscope/energy disperse spectroscopy that the testing sample after heat ageing is detected;
Kind and the content of objectionable impurities is determined according to testing result.
The detection method of objectionable impurities in transformator copper conductor the most according to claim 1, it is characterised in that utilize and sweep Retouch ultramicroscope/energy disperse spectroscopy the sample after heat ageing is detected, including:
Utilize scanning electron microscope that testing sample surface microscopic topographic is detected, determine the position of etch pit;
Utilize the X-ray energy spectrum of energy disperse spectroscopy capture etch pit interior element;
X-ray energy spectrum analytic process is used to determine etch pit interior element kind and content.
The detection method of objectionable impurities in transformator copper conductor the most according to claim 1, it is characterised in that described general Testing sample after immersion oil loads in described conical flask, including:
Testing sample after immersion oil is inserted in described conical flask, and keeps described testing sample to lie against the bottle of described conical flask At at the end.
The detection method of objectionable impurities in transformator copper conductor the most according to claim 1, it is characterised in that described newly Transformer oil is the transformer oil not containing active sulfur compound and sulfur content less than or equal to 1000ppm.
The detection method of objectionable impurities in transformator copper conductor the most according to claim 1, it is characterised in that state to be measured Sample is transformator copper conductor, and the shape of described testing sample is uniform.
The detection method of objectionable impurities in transformator copper conductor the most according to claim 1, it is characterised in that described two The concentration of benzyl two sulfur is 200-10000ppm.
The detection method of objectionable impurities in transformator copper conductor the most according to claim 1, it is characterised in that described heat Ageing time is 50-1000 hour.
The detection method of objectionable impurities in transformator copper conductor the most according to claim 1, it is characterised in that described very Temperature in empty ageing oven is set to 120 °-200 °.
CN201610677322.9A 2016-08-17 2016-08-17 The detection method of objectionable impurities in a kind of transformator copper conductor Pending CN106198588A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110291674A1 (en) * 2009-04-07 2011-12-01 Noboru Hosokawa Apparatus and method for analyzing the state of oil-filled electrical devices
CN105136550A (en) * 2015-09-11 2015-12-09 云南电网有限责任公司电力科学研究院 Method of checking harmful impurities in copper conductor for transformer
CN105223217A (en) * 2015-09-11 2016-01-06 云南电网有限责任公司电力科学研究院 The method that in detecting insulating oil, active sulfur compound exists in situation is there is based on oxygen
CN105699417A (en) * 2016-01-25 2016-06-22 云南电网有限责任公司电力科学研究院 Characterization method for corrosive sulfur of transformer insulating oil

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110291674A1 (en) * 2009-04-07 2011-12-01 Noboru Hosokawa Apparatus and method for analyzing the state of oil-filled electrical devices
CN105136550A (en) * 2015-09-11 2015-12-09 云南电网有限责任公司电力科学研究院 Method of checking harmful impurities in copper conductor for transformer
CN105223217A (en) * 2015-09-11 2016-01-06 云南电网有限责任公司电力科学研究院 The method that in detecting insulating oil, active sulfur compound exists in situation is there is based on oxygen
CN105699417A (en) * 2016-01-25 2016-06-22 云南电网有限责任公司电力科学研究院 Characterization method for corrosive sulfur of transformer insulating oil

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