CN103149229A - Method for detecting material compositions and contents thereof of welding material - Google Patents

Method for detecting material compositions and contents thereof of welding material Download PDF

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Publication number
CN103149229A
CN103149229A CN2013100680960A CN201310068096A CN103149229A CN 103149229 A CN103149229 A CN 103149229A CN 2013100680960 A CN2013100680960 A CN 2013100680960A CN 201310068096 A CN201310068096 A CN 201310068096A CN 103149229 A CN103149229 A CN 103149229A
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China
Prior art keywords
welding
welding material
sample
different
content
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Pending
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CN2013100680960A
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Chinese (zh)
Inventor
曾令熙
宋宝瑞
朱志敏
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SICHUAN HANLONG NEW MATERIALS CO Ltd
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SICHUAN HANLONG NEW MATERIALS CO Ltd
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Priority to CN2013100680960A priority Critical patent/CN103149229A/en
Publication of CN103149229A publication Critical patent/CN103149229A/en
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Abstract

The invention discloses a method for detecting material compositions and contents thereof of a welding material. The method comprises the steps of quantitatively taking a welding material sample, sufficiently dissociating the welding material, carrying out sample splitting and observing a sample appearance on an observation instrument; and carrying out chemical ingredient analysis on different particles through an energy spectrum, determining the material compositions, carrying out size grading, counting the sizes of the array areas of different material particles, and determining content of each material according to the densities and the distribution areas of the different materials. Shown by the detection, the welding material comprises the following material compositions in percentage by weight: 31% of marble, 15% of fluorite, 9% of ferrotitanium, 7% of low-carbon silicon iron, 5% of mid-carbon ferromanganese, 8% of titanium dioxide, 4% of nickel powder, 7% of tungsten carbide, 4% of mica, 1.2% of sodium carbonate, 3% of CeO2, 3% of Al2O3, 1.5% of K2O and 1.3% of Na2O. The method for detecting the material compositions and the contents thereof of the welding material provided by the invention has an accurate and comprehensive detection result.

Description

The detection method of welding material material composition and content thereof
Technical field
The present invention relates to a kind of technical field of welding materials, the detection method of specifically a kind of oxidation-containing cerium welding rod, and a kind of welding material material composition and content thereof.
Background technology
Welding material mainly comprises: the core wire of electrode coating, flux cored wire, hide the solder flux, the slag of electroslag welding of weldering etc.Wherein, welding rod is made of coating and core wire, and coating mainly plays mechanical protection effect and gas protective effect, Metallurgical processing effect and improves welding technological properties, is one of principal element that determines the weld metal quality.Select different arc stabilizers, slag former, gas-forming agent, deoxidizer, cementing agent, forming agent etc. according to the different needs of welding material, these all reach by controlling the different composition variations of coating.Yet the constituent of coating is complicated, is the potpourri of multiple different material.Vital role due to coating in welding process, therefore, compositions of surfacing metal is formed and detects is the important step of production quality control in the welding rod production run always.
The typical low-alloy steel electrodes such as existing E5515 type are when welding carbon equivalent ce〉during the Hi-Stren steel such as 0.4% medium carbon steel and Q390, for avoiding producing hardened structure and crackle, need adopt special technological measure during welding, as weld preheating to 250 ℃~400 ℃, adopt thin welding rod, little electric current to reduce the depth of fusion of mother metal, slow down the cooling velocity of heat-affected zone; Postheating and carry out stress relief annealing etc.Increase the production cycle in the middle of this is invisible, increased production cost.Although this type of welding rod price is low, performance is low, and production cost is high.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, and a kind of welding material is provided, and does not need preheating before weldering, need not adopt thin welding rod, little electric current, and postwelding does not need to carry out stress relief annealing, has shortened the production cycle, has reduced production cost.Provide simultaneously the detection method of a kind of welding material material composition and content thereof, to not accurate enough, the comprehensive problem of testing result in prior art to be solved.
For solving above-mentioned technical matters, the present invention by the following technical solutions:
The detection method of a kind of welding material material composition and content thereof comprises that getting 3 different batches samples detects separately respectively, and described detection method is further comprising the steps of:
A. the coating that dissociates, the described coating that dissociates make between the different constituents of coating and dissociate, and adopt agate mortar to grind, and milling time is controlled at 10 to 20 minutes;
B. ultrasonic Separation, described ultrasonic Separation are separated the different material of parcel adhesion, and the ultrasound wave frequency of operation is 40 KHz, and the working time is 45 to 60 minutes;
C. be 3 equal portions with sample splitting, carry out respectively sample topography and observe on optical viewer; Variable grain is carried out the power spectrum chemical composition analysis, determine that material forms; Grain size segregation, statistics different material granule number level size is determined each content of material according to density and the distribution area thereof of different material; Through detecting, the material of described welding material forms and weight percent content is: marble 35%, fluorite 15%, ferrotianium 9%, low-carbon ferrosilicon 7%, mid-carbon fe-mn 5%, titanium dioxide 8%, tungsten carbide 7%, mica 4%, soda ash 1.2%, CeO 2Be 3%, Al 2O 33%, K 2O1.5%, Na 2O1.3%.
Further technical scheme is that grain size segregation comprises: sieve method, elutriation method.
Further technical scheme is that the medium of ultrasonic Separation is selected from a kind of in ethanol, acetone.
Compared with prior art, one of beneficial effect of the present invention is: do not need preheating before the welding material weldering, need not adopt thin welding rod, little electric current, postwelding does not need to carry out stress relief annealing, has shortened the production cycle, has reduced production cost.In addition, welding material is directly processed, adopted structure, the constituent do not destroy the welding material construct, can choose independent phase and analyze due to micro-zone analysis, avoided the many materials of chemical analysis to mix the impact of the heterogeneity that causes; Material by micro-zone analysis direct-detection welding material forms and granule size, reaches not only to determine its chemical composition but also determine its existence form, satisfies the meticulous detection of welding rod material quality, thereby guarantees the consistance of high-quality wlding.
Description of drawings
Fig. 1 is that the fluorite of sample in one embodiment of the invention is measured the energy spectrogram.
Embodiment
The present invention is further elaborated below in conjunction with accompanying drawing.
The detection method of one embodiment of the invention welding material material composition and content thereof, detecting step is: the welding material laboratory sample of choosing three different batches, welding material can be electrode coating, flux cored wire core wire, hide the solder flux, the welding materials such as slag of electroslag welding of weldering, as specific embodiment, the welding material of the present embodiment is chosen the welding material that the oxidation-containing cerium welding rod detects as the present embodiment.But and be not understood to the uniqueness restriction that butt welding connects material selection.The present embodiment is peeled off covering of an electrode and core wire by adopting mechanical means with three different batches welding rods, obtains coating weight 500 grams, the welding material sample of three different batches is preserved separately respectively, and be also to detect separately respectively during detection.Get the welding material sample of one of them batch, the welding material sample is placed on gently to grind between different constituents in agate mortar fully dissociates.The sample that fully dissociates after grinding is put into 1000 ml beakers, heat appropriate medium, medium can be that acetone can be also ethanol, the present embodiment medium is ethanol, sample is put into ultrasonic container, the parcel adhesion between the ultrasonic Separation different material, in the present embodiment, hyperacoustic frequency of operation is 40 KHz, working time is at 45 to 60 minutes, preferably 50 minutes.Taking-up is put into baking oven with the sample that has fully dissociated and is dried by the sample of ultrasonic Separation, weighs, and sample preparation; Sample is carried out morphology observation, and after sample splitting became 10 grams, can select sample is evenly spread upon magnitude range was on the conducting adhesive cloth of 2 square millimeters to 5 square millimeters, and specific embodiment is that sample is evenly spread upon on the conducting adhesive cloth of 3 square millimeters; With the sample surfaces plating carbon that spreads upon on conducting adhesive cloth; The sample that spreads upon conducting adhesive cloth upper surface plating carbon is put into scanning electron microscope, carry out sample topography and observe, optical viewer can be transmission electron microscope, scanning electron microscope etc., and as preferred embodiment, in the present embodiment, optical viewer is scanning electron microscope.Adopt scanning electron microscope to carry out morphology observation to sample, in scanning electron microscope, not only can utilize the interaction of incident electron and sample to produce various information and come imaging, and can pass through signal processing method, obtain the Special Display Method of multiple image, can also obtain many-sided data from the surface topography of sample.Because the scanning electron picture does not record simultaneously, it is decomposed into nearly 1,000,000 and successively records according to this formation.Thereby make scanning electron microscope can also carry out the analysis of composition and element except observing surface topography.Next step is grain size segregation, and grain size segregation can adopt sieve method or elutriation method, and wherein sieve method is to detect with sieve the technology that raw meal particle size forms, and is one of important method of raw meal particle size analysis, is called for short screen analysis.The particle size range of screen analysis is 300~0.045mm.Coarse grain (screen analysis of 300~6mm) the materials sieve of punching steel plate or gauze fabric, particulate (6~0.045mm) material normal test sieves.According to detecting needs, select the screen cloth of different size of mesh during screen analysis, form bushing screen.The required sample quality of screen analysis can be chosen by tabular numerical value; Also can calculate by empirical formula.Elutriation method is the settling velocity difference of particle in flowing water or hydrostatic according to different thicknesses, a kind of Analytical Methods of Grain Grade that material is divided into groups.As specific embodiment, in the present embodiment, grain size segregation adopts sieve method.Statistics different material granule number level size is determined each content of material according to density and the distribution area thereof of different material.Variable grain is carried out the power spectrum chemical composition analysis, can choose independent phase and analyze due to micro-zone analysis, avoided the many materials of chemical analysis to mix the impact of the heterogeneity that causes.By the spectroscopy detection to material composition, make the standard spectrogram of late detection comparison; By the spectroscopy detection contrast raw material collection of illustrative plates to individual each particle of grade, the material that obtains a grade forms.Each particle is measured one by one, then to the amount of measuring add up and there emerged a the content of composition.Said determination is completed on FEI-Quanta250SEM scanning electron microscope and EDAX-genesis energy spectrometer.The accelerating potential of scanning electron microscope is 25kv, and Spot Size is 7.0.The Amp times of energy spectrometer is 6.4; Cps is 26000; DT% is 30%.Three batches are detected respectively.
Adopting the present embodiment method can accurately obtain chief component composition situation of change in sample, can more completely reflect the particle size distribution situation of sample simultaneously, is an important means of the quality guarantee of welding material.
As shown in Figure 1, Fig. 1 shows the fluorite of sample in the present embodiment and measures the energy spectrogram, and the mensuration that in figure, also not shown all substances form can spectrogram.Through detecting, in the present embodiment, welding material sample material composition and content thereof are (% by weight): marble 35%, fluorite 15%, ferrotianium 9%, low-carbon ferrosilicon 7%, mid-carbon fe-mn 5%, titanium dioxide 8%, tungsten carbide 7%, mica 4%, soda ash 1.2%, CeO 2Be 3%, Al 2O 33%, K 2O1.5%, Na 2O1.3%.
" embodiment " who speaks of in this manual, " another embodiment ", " embodiment ", etc., refer to specific features, structure or the characteristics described in conjunction with this embodiment and be included at least one embodiment that the application's generality describes.A plurality of local appearance statement of the same race is not necessarily to refer to same embodiment in instructions.Furthermore, when describing a specific features, structure or characteristics in conjunction with any embodiment, what advocate is to realize that in conjunction with other embodiment this feature, structure or characteristics also fall within the scope of the invention.
Although invention has been described with reference to a plurality of explanatory embodiment that invents here, but, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and within embodiment will drop on the disclosed principle scope and spirit of the application.More particularly, in the scope of, accompanying drawing open in the application and claim, can carry out multiple modification and improvement to building block and/or the layout of subject combination layout.Except modification that building block and/or layout are carried out with improving, to those skilled in the art, other purposes will be also obvious.

Claims (3)

1. a welding material material forms and the detection method of content, comprises that getting 3 different batches samples detects separately respectively, and it is characterized in that: described detection method is further comprising the steps of:
A. the coating that dissociates, the described coating that dissociates make between the different constituents of coating and dissociate, and adopt agate mortar to grind, and milling time is controlled at 10 to 20 minutes;
B. ultrasonic Separation, described ultrasonic Separation are separated the different material of parcel adhesion, and the ultrasound wave frequency of operation is 40 KHz, and the working time is 45 to 60 minutes;
C. be 3 equal portions with sample splitting, carry out respectively sample topography and observe on optical viewer; Variable grain is carried out the power spectrum chemical composition analysis, determine that material forms; Grain size segregation, statistics different material granule number level size is determined each content of material according to density and the distribution area thereof of different material; Through detecting, the material of described welding material forms and weight percent content is: marble 35%, fluorite 15%, ferrotianium 9%, low-carbon ferrosilicon 7%, mid-carbon fe-mn 5%, titanium dioxide 8%, tungsten carbide 7%, mica 4%, soda ash 1.2%, CeO 2Be 3%, Al 2O 33%, K 2O1.5%, Na 2O1.3%.
2. the detection method of welding material material composition according to claim 1 and content thereof, is characterized in that described grain size segregation comprises: sieve method, elutriation method.
3. welding material material according to claim 1 forms and the detection method of content, and the medium that it is characterized in that described ultrasonic Separation is a kind of in ethanol, acetone.
CN2013100680960A 2013-03-04 2013-03-04 Method for detecting material compositions and contents thereof of welding material Pending CN103149229A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111766203A (en) * 2020-07-15 2020-10-13 龙游岛式智能科技有限公司 Welding electrode coating defect and firm filling detection device
CN112059469A (en) * 2018-11-28 2020-12-11 东莞理工学院 Preparation method of submerged-arc welding flux-cored wire

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JP2003130786A (en) * 2001-10-23 2003-05-08 Dainippon Ink & Chem Inc Method for evaluating particles in printing ink
FR2851933A1 (en) * 2003-03-03 2004-09-10 Gaston Bayourthe Filter to retain solid particles in liquid samples, of fruit juices and especially grape must for chemical and molecular analysis, is a cylindrical tube with a lower outlet disk closure and a bent upper rim to hold the filter structures
CN101121544A (en) * 2006-08-11 2008-02-13 李大楠 Synthesized high mercury compound and preparation method thereof
CN101491694A (en) * 2009-03-03 2009-07-29 陕西科技大学 Preparation method of carbon fibre reinforced hydroxylapatite composite material
CN102500255A (en) * 2011-10-31 2012-06-20 中国科学院苏州纳米技术与纳米仿生研究所 Carbon nano tube dispersing method
CN102818723A (en) * 2012-09-07 2012-12-12 首钢总公司 Method of electrolytically extracting and detecting fine inclusions in steel

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1337295A (en) * 2001-08-11 2002-02-27 无锡威孚吉大新材料应用开发有限公司 Nano metal solder and its prepn
JP2003130786A (en) * 2001-10-23 2003-05-08 Dainippon Ink & Chem Inc Method for evaluating particles in printing ink
FR2851933A1 (en) * 2003-03-03 2004-09-10 Gaston Bayourthe Filter to retain solid particles in liquid samples, of fruit juices and especially grape must for chemical and molecular analysis, is a cylindrical tube with a lower outlet disk closure and a bent upper rim to hold the filter structures
CN101121544A (en) * 2006-08-11 2008-02-13 李大楠 Synthesized high mercury compound and preparation method thereof
CN101491694A (en) * 2009-03-03 2009-07-29 陕西科技大学 Preparation method of carbon fibre reinforced hydroxylapatite composite material
CN102500255A (en) * 2011-10-31 2012-06-20 中国科学院苏州纳米技术与纳米仿生研究所 Carbon nano tube dispersing method
CN102818723A (en) * 2012-09-07 2012-12-12 首钢总公司 Method of electrolytically extracting and detecting fine inclusions in steel

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112059469A (en) * 2018-11-28 2020-12-11 东莞理工学院 Preparation method of submerged-arc welding flux-cored wire
CN111766203A (en) * 2020-07-15 2020-10-13 龙游岛式智能科技有限公司 Welding electrode coating defect and firm filling detection device
CN111766203B (en) * 2020-07-15 2021-03-09 宋小梅 Welding electrode coating defect and firm filling detection device

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Inventor after: Zeng Lingxi

Inventor after: Cao Jia

Inventor after: Song Baorui

Inventor after: Guo Ping

Inventor after: Huang Peng

Inventor before: Zeng Lingxi

Inventor before: Song Baorui

Inventor before: Zhu Zhimin

COR Change of bibliographic data

Free format text: CORRECT: INVENTOR; FROM: CENG LINGXI SONG BAORUI ZHU ZHIMIN TO: CENG LINGXI CAO JIA SONG BAORUI GUOPING HUANG PENG

C12 Rejection of a patent application after its publication
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Application publication date: 20130612