CN100578198C - Be used to detect stainless spectral standard sample of coinage and manufacture method thereof - Google Patents
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Abstract
The present invention relates to a kind of stainless steel optical spectrum standard model, especially for detecting stainless spectral standard sample of coinage and manufacture method thereof, be by impurity element carbon, silicon, manganese, phosphorus, sulphur and interpolation element boron, nickel, copper, chromium, with iron is that base-material calculates various raw material additions by formulation ratio, raw material is added founding processing in the vacuum induction smelting furnace, furnace charge melted 95% o'clock, materials and do total analysis, adjust the molten steel chemical constitution according to chemical analysis results, ferro-boron was put into ingot mould in advance with ferrosilicon adjustment silicone content in 7-10 minute before the tapping; After treating that each elemental composition meets the demands, control tapping temperature: 1520-1540 ℃, pour molten steel into ingot mould, stamp sample number after the cooling respectively.Standard sample for spectrochemical analysis good uniformity of the present invention, combined content wide ranges, element kind are many, preparation technology advanced person, and definite value is accurate, and concentration gradients rationally makes it obviously be better than domestic and international similar standard specimen in analyzing domestic coinage stainless steel material.
Description
Technical field
The present invention relates to a kind of stainless steel optical spectrum standard model, especially for detecting stainless spectral standard sample of coinage and manufacture method thereof.
Background technology
With the coin that stainless steel is made, not only its silvery white metallic luster has certain sight, and performance index such as it is corrosion-resistant, fastness all are better than copper alloy coin, and cost is lower than the latter again.The coin that stainless steel is all arranged in the coin series of therefore many in the world countries distribution, for maintaining secrecy and aspect factor such as false proof, the chemical constitution of the stainless steel that various countries adopt all is not quite similar.Renminbi never has the coin kind of stainless steel for a long time, at this situation, through a large amount of investigation, China Banknote Primting and Minting Corporation has developed new China's first kind of coinage special stainless steel alloy in 2004, this is a kind of and other national coinage with the stainless steel novel coinage stainless steel different with civilian stainless steel.For the chemical constitution of assurance product and the content of special security element, also, must adopt convenient, accurate, high efficiency spectral instrument that the chemical constitution of product is analyzed for satisfying the needs of both analysis.And standard sample for spectrochemical analysis consistent with the matrix of detected sample be to guarantee analysis result prerequisite accurately and reliably, so a cover and the spectral analysis standard model that this coinage stainless steel matrix is complementary must be arranged, could guarantee above-mentioned detection quality.By retrieving relevant patent and document both at home and abroad, the relevant stainless steel optical spectrum standard specimen of Britain, the relevant stainless steel optical spectrum standard specimen of Japan and the Cr13 standard sample for spectrochemical analysis of domestic GBW01605-01609 thereof, the stainless steel optical spectrum standard specimen of GSBA68001-68007, the stainless steel optical spectrum standard specimen of GSBH400115-1996 are analyzed, find above standard sample for spectrochemical analysis have following some be not suitable for analyzing domestic coinage stainless steel material: 1. be not inconsistent with domestic coinage stainless steel material matrix; 2. security element B can't detect; 3. other constituent content distributes undesirable etc.In a word, at present the stainless steel optical spectrum standard model on the domestic and international market is basically in the face of civilian stainless steel product and develop, and narrow application range, can not satisfy all conditions that domestic coinage stainless steel is analyzed needs simultaneously.For these reasons, a cover must be made and the needs that corresponding coinage is produced could be satisfied with the spectral analysis standard model that this coinage stainless steel material matrix is complementary.
Summary of the invention
The object of the present invention is to provide a kind of detection spectral standard sample that is complementary with stainless steel with China's coinage, for the check fast and accurately that realizes coinage stainless steel founding production, finished product provides necessary condition, guarantee that product quality satisfies coinage and produces needs, and can be used for the detection that multiple trade mark stainless steel comprises the coinage stainless steel alloy.
Another object of the present invention provides a kind of method of making described stainless steel detection with spectral standard sample.
The spectral standard sample that is used for the detection of coinage stainless steel of the present invention is by impurity element carbon, silicon, manganese, phosphorus, sulphur and interpolation element boron, nickel, copper, chromium, is base-material with iron, and % is as follows by weight:
Carbon: 0.0022%～0.091%
Silicon: 0.046%～1.18%
Manganese: 0.123%～1.20%
Phosphorus: 0.0049%～0.053%
Sulphur: 0.0041%～0.036%
Boron: 0.0008%～0.064%
Chromium: 13.93%～20.24%
Nickel: 0.052%～0.91%
Copper: 0.048%～0.51%
Iron: surplus.
The present invention is owing to contained component complexity, content range fusing point wide, element in addition, boiling point differ bigger, some element is because deoxidation is easy to loss, it is very big influenced by smelting time, easily produces segregation, and it is promptly overall uneven that low-melting element often shows as orderly segregation; The element that has solubleness in iron and steel is very low, and it is promptly local uneven to be usually expressed as unordered segregation, and this just constitutes technological difficulties of the present invention.Corresponding technical measures must be taked for this reason, intermediate alloy must be prepared as element boron; Easily slag making in melting must be adopted vacuum casting or carry out necessary gas shield; And for example phosphorus, sulphur etc. are subjected to factor affecting such as melting furnace kind, smelting time, temperature, atmospheric condition very big, therefore melted 95% o'clock at furnace charge, total analysis is done in sampling, adjusts molten steel, adjusts the content of manganese, chromium, carbon, phosphorus, sulphur and adjusted silicone content, ferro-boron with ferrosilicon in 7-10 minute and put into a series of technical measures such as ingot mould in advance and guaranteed before tapping according to its result.Make its trade mark stainless steel alloy analyzing and testing of will being correlated be blended in a cover spectral standard sample both at home and abroad, to realize being suitable for many trades mark stainless steel product testing goal.But increased the difficulty that standard specimen preparation, valued methods are selected.
Method of the present invention is designed to the content distribution of gradient to 9 elements in the standard model, and matrix element iron is surplus.So just guaranteed both to have can be used for same standard model in the actual analysis impurity analysis of direct reading spectrometry, simultaneously also can be used for Xray fluorescence spectrometer analyzes the chromium element of high-load, not only reduce expenses but also also have obvious advantages technically, more satisfy demand of practical production.
Various factors in the comprehensive real work, this standard model comprises 7 points, can make carbon, silicon, manganese, phosphorus, sulphur, boron, nickel, copper, chromium totally 9 working curves that element is complete at 1～5, and 6,7 are designed to the height mark, both can participate in working curve and make, and can independently carry out standardization again and proofread and correct.Proofread and correct because routine work only needs 6,7 two standard specimens of grinding to carry out standardization, 1～5 loss is very little; Finish using when 6,7 two, can in 1～5, reselect high substandard and carry out standardization effort.Thereby improve twice the serviceable life that can make this spectral standard sample, obviously reduce use cost.
The present invention makes the method for this standard model, comprises following processing step:
A), the batching founding processing of selecting materials: each component is calculated various raw material additions by formulation ratio, raw material iron, copper, nickel, manganese, chromium etc. are added in the vacuum induction smelting furnace, its capacity is 100 kilograms, power 100KW, 6-8 minute supply 60% power begins to switch on, gradually power is risen to maximal value, note smashing material at any time with the furnace charge fusing.When furnace charge melted 95%, total analysis was done in sampling, adjusted the molten steel chemical constitution according to analysis result, at reduction period with ferromanganese, ferrochrome, adjustment manganese, chromium content; Adjust carbon, phosphorus, sulfur content with the pig iron, graphite electrode fragment, coke fragment; Adjusted silicone content with Antaciron in 7-10 minute before the tapping, ferro-boron is put into ingot mould in advance, will carry out chemical composition analysis to respective element between the adjustment period of composition.
B), treat that each elemental composition meets the demands after, control tapping temperature: 1520-1540 ℃, ingot mould is heated to 500-700 ℃ in advance, stamps sample number respectively after pouring molten steel cools into.
Described raw material iron, copper, nickel, manganese, chromium are respectively pure iron, cathode copper, electrolytic nickel, electrolytic manganese and pure chromium; Ferromanganese, ferrochrome, the pig iron, graphite electrode fragment, coke fragment, ferro-boron are modified raw material.
The present invention compared with prior art, because the design of this standard model is fully according to GB/T15000-94 " standard model work guide rule ", JJG1006-94 " primary standard material technical manual ", the requirement of YB/T082-1996 " metallurgic product analysis standard model technical manual " is carried out, whole fabrication scheme is by composition and content design, select materials and prepare burden, founding, preanalysis, the institutional framework check of casting rod, uniformity testing, definite value, data processing, determining of standard value and standard deviation, examination is checked and produced to spectral analysis curve " linear ", comparison with domestic and international similar standard model level, a series of processes such as stability inspection prove, standard sample for spectrochemical analysis good uniformity of the present invention, the combined content wide ranges, the element kind is many, not only satisfy standard-required, being suitable for domestic coinage stainless steel detects, overlap in the spectral standard sample but also the trade mark stainless steel alloy analyzing and testing of will being correlated with both at home and abroad is melted into one, many trades mark stainless steel product is detected thereby this standard model is suitable for.Simultaneously improved twice the serviceable life of standard specimen, obviously reduce use cost, satisfy demand of practical production; This standard specimen is reasonable in design, preparation technology is advanced, makes contained 9 elements become equal difference to distribute, definite value accurately and reliably, concentration gradients rationally causes it obviously to be better than domestic and international similar standard specimen in analyzing domestic coinage stainless steel material.
Embodiment
The present invention further specifies summary of the invention by embodiment, but not limit by embodiment.
Embodiment 1: by the weight % of component concentration: carbon less than 0.02, silicon 0.06, manganese 0.15, phosphorus less than 0.01, sulphur 0.006, nickel 0.70, copper 0.06, chromium 19.0, boron 0.0008, iron surplus calculates pure iron as raw material, cathode copper, electrolytic nickel, electrolytic manganese and pure network and adds in the vacuum induction smelting furnace, its capacity is 100 kilograms, power 100KW, 6-8 minute supply 60% power begins to switch on, after treating that rush of current stops, gradually power is risen to maximal value, smash material at any time with the furnace charge fusing.Furnace charge melted 95% o'clock, total analysis is done in sampling, adjust the molten steel chemical constitution according to analysis result, at reduction period with ferromanganese, ferrochrome, adjustment manganese, chromium content, adjust carbon, phosphorus, sulfur content with the pig iron, graphite electrode fragment, coke fragment, ferro-boron was put into ingot mould in advance with Antaciron adjustment silicone content in 7-10 minute before the tapping; After treating that each elemental composition meets the demands, the control tapping temperature is at 1520-1540 ℃, and ingot mould is heated to 500-700 ℃ in advance, stamps sample number after pouring molten steel into cooling.
Embodiment 2-7 and embodiment 1 are except that the component concentration change of each stove, and be all identical with embodiment 1.
| Embodiment | C (％) | Si (％) | Mn (％) | P (％) | S (％) | Ni (％) | Cu (％) | Cr (％) | B (％) | Fe (％) |
| 2 | 0.04 | 0.40 | 0.58 | 0.015 | 0.013 | 0.90 | 0.12 | 18.0 | 0.0015 | Surplus |
| 3 | 0.06 | 0.65 | 0.90 | 0.026 | 0.021 | 0.45 | 0.25 | 17.0 | 0.006 | Surplus |
| 4 | 0.09 | 1.00 | 1.10 | 0.038 | 0.026 | 0.05 | 0.35 | 16.0 | 0.013 | Surplus |
| 5 | 0.08 | 1.10 | 1.20 | 0.050 | 0.031 | 0.18 | 0.50 | 15.0 | 0.060 | Surplus |
| 6 | 0.03 | 0.25 | 0.45 | 0.015 | 0.008 | 0.78 | 0.15 | 20.0 | 0.0035 | Surplus |
| 7 | 0.08 | 0.85 | 1.00 | 0.052 | 0.036 | 0.18 | 0.45 | 14.0 | 0.064 | Surplus |
This standard specimen of producing with the inventive method just can be used for producing after the qualified and definite value analysis through uniformity testing respectively.Branch is chatted as follows:
1. uniformity testing:
Spectral standard sample requires the chemical content of each element all can keep composition even vertically reaching on each point of square section of casting rod, and segregation-free produces.
Concrete checkout procedure is: after the standard specimen founding is finished, will cast rod and cut the mouth of a river, and strand be taken a sample end to end carry out chemical constitution segregation check; Be processed into Φ 55mm round steel through forging after the assay was approved, forging stub bar tail sampling carrying out physics macroscopic examination once more; After determining that steel better, will forge with lathe that expecting strips off the skin is polished into Φ 35 ± 2mm round steel, and cut into the right cylinder of high 50 ± 3mm; High photo-electric direct reading spectrometer and the Xray fluorescence spectrometer of precision adopted in 10 of random samplings once more, analytical element done uniformity coefficient measure, and repeats 3 times." range method " by the spectral standard sample uniformity testing judged.By the homogeneity of the comparison judgement sample of extreme difference in extreme difference between group and the group, setting R is a statistic, and R0 is the statistic critical value, if all elements R＜R0, then the founding of decidable sample is even.
2. definite value analysis:
Adopt inspection machines such as ICP and infrared carbon sulphur instrument, analytical approach is selected is classical way in the corresponding content range of each element mostly, according to the current techique standard, and by 8 tame unit independent analysis, i.e. every every element 8 groups of value data altogether.Every group comprises 4 data, constituent parts all use two or more methods or more than two the person of analysing finish, overcome method and human factor error.Like this, every of this standard model every element has 32 value data.Quantitatively can be to guarantee definite value result's accuracy.More than various measures fundamentally eliminated deviation and the mistake that may introduce.
Selecting for use of definite value chemical analysis method is reliable:
Because of sample component complexity, very big to standard model definite value accuracy influence, select reliable analytical method very important, the definite value analytical approach that following table adopts for each element.
| Element | Analytical approach |
| C | Gas volumetric method after the tubular furnace internal combustion; The high-frequency combustion infrared absorption |
| Si | Perchloric acid dehydrated weight method; The ICP-AES method; Reduced form silicomolybdate photometry |
| Mn | The potassium metaperiodate photometry; The ICP-AES method; Ammonium persulfate oxidation photometry |
| P | The n-butyl acetate extraction photometry; Antimony phosphorus molybdenum blue spectrophotometry; The ICP-AES method; Bismuth phosphorus molybdenum blue spectrophotometry; Normal butyl alcohol-chloroform extraction photometry |
| S | The high-frequency combustion infrared absorption; Aluminium oxide stratography barium sulphate gravimetric method |
| Cr | The ammonium persulfate oxidimetry; The ICP-AES method |
| Ni | The ICP-AES method; The dimethylglyoxime photometry; |
| Cu | New cuprous spirit-chloroform extraction photometry; The ICP-AES method; The bisoxalydihydrazone photometry |
| B | Methylene blue-1,2-ethylene dichloride extraction spectrophotometric method; The ICP-AES method |
Through relatively, can draw that coinage is reasonable in design with the stainless steel optical spectrum standard model, preparation technology is advanced, make carbon, silicon, manganese, phosphorus, sulphur, boron, chromium, nickel, 9 elements of copper become equal difference to distribute, definite value accurately and reliably, concentration gradients distributes rationally.Can be satisfied with photo-electric direct reading spectrometer and Xray fluorescence spectrometer simultaneously and analyze requirement, can be used for measuring domestic coinage whole elements in the stainless steel, the analyzing and testing scope of this standard model has also covered internal and international multiple coinage stainless steel material, obviously is better than domestic and international similar standard model.
The parameter designing of this cover standard model is than other similar standard model complexity, and the processing technology difficulty is big, thereby can embody higher technical merit.
Claims (10)
1, be used to detect the stainless spectral standard sample of coinage, it is characterized in that by impurity element carbon, silicon, manganese, phosphorus, sulphur, interpolation element boron, nickel, copper, chromium, and form as the iron of base-material, percentage by weight is as follows:
Carbon: 0.0022%～0.091%
Silicon: 0.046%～1.18%
Manganese: 0.123%～1.20%
Phosphorus: 0.0049%～0.053%
Sulphur: 0.0041%～0.036%
Boron: 0.0008%～0.064%
Chromium: 13.93%～20.24%
Nickel: 0.052%～0.91%
Copper: 0.048%～0.51%
Iron: surplus.
2, spectral standard sample according to claim 1 is characterized in that by impurity element, adds element and form as the iron of base-material, and percentage by weight is as follows:
Carbon＜0.02% silicon 0.06%
Manganese 0.15% phosphorus＜0.01%
Sulphur 0.006% nickel 0.70%
Copper 0.06% boron 0.0008%
Chromium 19.0% iron surplus.
3, spectral standard sample according to claim 1 is characterized in that by impurity element, adds element and form as the iron of base-material, and percentage by weight is as follows:
Carbon 0.04% silicon 0.4%
Manganese 0.58% phosphorus 0.015%
Sulphur 0.013% nickel 0.9%
Copper 0.12% boron 0.0015%
Chromium 18.0% iron surplus.
4, spectral standard sample according to claim 1 is characterized in that by impurity element, adds element and form as the iron of base-material, and percentage by weight is as follows:
Carbon 0.06% silicon 0.65%
Manganese 0.9% phosphorus 0.026%
Sulphur 0.021% nickel 0.45%
Copper 0.25% boron 0.006%
Chromium 17.0% iron surplus.
5, spectral standard sample according to claim 1 is characterized in that by impurity element, adds element and form as the iron of base-material, and percentage by weight is as follows:
Carbon 0.09% silicon 1.00%
Manganese 1.10% phosphorus 0.038%
Sulphur 0.026% nickel 0.05%
Copper 0.35% boron 0.013%
Chromium 16.0% iron surplus.
6, spectral standard sample according to claim 1 is characterized in that by impurity element, adds element and form as the iron of base-material, and percentage by weight is as follows:
Carbon 0.08% silicon 1.10%
Manganese 1.20% phosphorus 0.05%
Sulphur 0.031% nickel 0.18%
Copper 0.50% boron 0.06%
Chromium 15.0% iron surplus.
7, spectral standard sample according to claim 1 is characterized in that by impurity element, adds element and form as the iron of base-material, and percentage by weight is as follows:
Carbon 0.03% silicon 0.25%
Manganese 0.45% phosphorus 0.015%
Sulphur 0.008% nickel 0.78%
Copper 0.15% boron 0.0035%
Chromium 20.0% iron surplus.
8, spectral standard sample according to claim 1 is characterized in that by impurity element, adds element and form as the iron of base-material, and percentage by weight is as follows:
Carbon 0.08% silicon 0.85%
Manganese 1.00% phosphorus 0.052%
Sulphur 0.036% nickel 0.18%
Copper 0.45% boron 0.064%
Chromium 14.0% iron surplus.
9, the method for preparing the described spectral standard sample of claim 1 is characterized in that comprising following processing step:
A), the batching founding processing of selecting materials:
Each component is calculated various raw material additions by proportioning, with raw material iron, copper, nickel, manganese, chromium adds in the vacuum induction smelting furnace, its capacity is 100 kilograms, power 100KW, 6-8 minute supply 60% power begins to switch on, after treating that rush of current stops, gradually power is risen to maximal value, at any time note smashing material with the furnace charge fusing, furnace charge melted 95% o'clock, materialsed and did total analysis, adjusted the molten steel chemical constitution according to chemical analysis results, at reduction period with ferromanganese, ferrochrome is adjusted manganese, chromium content, with the pig iron, the graphite electrode fragment, the coke fragment is adjusted carbon, phosphorus, sulfur content, ferro-boron was put into ingot mould in advance with ferrosilicon adjustment silicone content in 7-10 minute before the tapping;
B), treat that each elemental composition meets the demands after, control tapping temperature: 1520-1540 ℃, ingot mould is heated to 500-700 ℃ in advance, and molten steel is poured into, stamps sample number after the cooling respectively.
10, the method for preparing spectral standard sample according to claim 9 is characterized in that described raw material iron, copper, nickel, manganese, chromium are respectively pure iron, cathode copper, electrolytic nickel, electrolytic manganese and pure chromium; Ferromanganese, ferrochrome, the pig iron, graphite electrode fragment, coke fragment, ferrosilicon, ferro-boron are modified raw material.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101398419B (en) * | 2008-11-04 | 2011-11-30 | 钢铁研究总院 | Concourse type metallurgy standard sample for minimal invasion analysis, preparation method and application thereof |
| CN102269665B (en) * | 2011-07-16 | 2012-10-03 | 山西百一机械设备制造有限公司 | Manufacturing method of master sample for nickel-containing pig iron spectral analysis |
| CN102590102A (en) * | 2012-02-21 | 2012-07-18 | 山东省冶金科学研究院 | Standard sample for spectroscopic analysis of welding wire steel ER50-6 |
| CN102721672A (en) * | 2012-06-05 | 2012-10-10 | 河北钢铁股份有限公司邯郸分公司 | Method for quickly measuring ultra-low carbon and ultra-low sulfur in steel by atomic emission spectrometry |
| CN102776451B (en) * | 2012-08-08 | 2014-04-16 | 山西太钢不锈钢股份有限公司 | Nickel-iron spectrum standard sample and preparation method thereof |
| CN103592324B (en) * | 2012-08-15 | 2016-05-25 | 南京造币有限公司 | For detection of signal bronze spectral standard sample and the manufacture method thereof of coinage coating |
| CN103115870A (en) * | 2013-01-28 | 2013-05-22 | 青岛云路新能源科技有限公司 | Laboratory preparation method of iron-base amorphous spectral standard sample |
| CN104359735B (en) * | 2014-11-14 | 2017-03-01 | 山西太钢不锈钢股份有限公司 | A kind of preparation method of high carbon stainless steel standard specimen |
| CN105004710B (en) * | 2015-07-27 | 2017-09-01 | 山西太钢不锈钢股份有限公司 | A kind of stainless steel chromium, nickel element analytic set method |
| CN105547777A (en) * | 2015-12-21 | 2016-05-04 | 本钢板材股份有限公司 | A preparing method of a pig iron standard sample |
| CN105606414A (en) * | 2015-12-21 | 2016-05-25 | 山东省冶金科学研究院 | A set of wire spectrum standard samples and preparation method |
| CN109030136B (en) * | 2018-06-21 | 2021-09-28 | 山西太钢不锈钢股份有限公司 | Preparation method of standard sample for 400 series stainless steel spectral analysis and standard sample |
| CN109872442B (en) * | 2019-02-15 | 2021-02-02 | 常州万泰天平仪器有限公司 | Coin detection method and system and coin weight detector |
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