CN102776451A - Nickel-iron spectrum standard sample and preparation method thereof - Google Patents
Nickel-iron spectrum standard sample and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nickel-iron spectrum standard sample and a preparation method thereof. The nickel-iron spectrum standard sample is characterized by comprising the following chemical elements by weight: 14.9-50.0% of Ni, 0.03-2.50% of C, 0.2-4.5% of Si, 0.004-0.040% of P, 0.002-0.300% of S, 0.4-2.0% of Co, 0.01-0.25% of Cu, 0.1-2.0% of Cr and 40-80% of Fe. The method utilizes processes including intermediate-frequency furnace smelting, rain drench type pouring, water cooling copper mould casting, tundish bottom pouring and the like, so that uniform component tissue of the spectrum standard sample is ensured.
Description
Technical field
The present invention relates to a kind of ferronickel standard model and preparation method thereof, belong to the metallurgical analysis field.
Background technology
At present, ferronickel is the important source material of products such as smelting stainless steel, nickel-base alloy, and production and use enterprise must have corresponding with it standard model to estimate and the check analysis quality in order to control the quality product of ferronickel, and calibration and drawing curve.All do not have the ferronickel spectral standard sample to be used for instrument at present both at home and abroad and draw and the correction work curve, brought inconvenience for the spectral measurement of ferronickel.Given this, design special process development one cover ferronickel standard model is used for spectrograph calibration and drawing curve.
Summary of the invention
The purpose of this invention is to provide a kind of ferronickel spectral standard sample that evenly contains nickel, iron and carbon, silicon, phosphorus, cobalt, copper, chromium, element sulphur.
Another object of the present invention provides the preparation method of this ferronickel spectral standard sample.
Ferronickel spectral standard sample described in the object of the invention through adopting special preparation technology, is effectively guaranteed this spectra sample structural state and homogeneity.
Ferronickel spectral standard sample provided by the invention is characterized in that: it evenly contains the chemical element of following weight per-cent:
Ni：14.9～50.0%；
C：0.03～2.50%；
Si：0.2～4.5%；
P：0.004～0.040%；
S：0.002～0.300%；
Co：0.4～2.0%；
Cu：0.01～0.25%；
Cr：0.1～2.0%；
Fe：40~80%；
Surplus is an impurity.
The preparation method of ferronickel spectral standard sample provided by the invention is characterized in that: may further comprise the steps:
(1) raw material being added intermediate frequency furnace smelts: adopt metallic nickel, ferrosilicon, the pig iron, carbon steel, pure iron, chromium metal, metallic copper, cobalt metal, metallic aluminium, ferrophosphorus, fluorite, lime as raw material, prepare burden by each constituent content of ferronickel spectral standard sample;
(2) adopt the formula cast that drenches with rain, the casting of water-cooled copper mould: gating system all adopts the pyroceramic goods, adopts the top mode that drenches with rain, and is even for guaranteeing composition, guarantees that no graphite carbon separates out, and adopts that copper mould is processed, manufacturing, water-cooled;
(3) adopt the tundish bottom pouring: molten steel changes tundish over to, and calm 10 minutes, open to water after 10 seconds and open water-in, water to finish and close water-in after 10 minutes, be incubated 45 minutes and take out standard sample for spectrochemical analysis;
(4) reconditioning, finishing and numbering: with sample reconditioning and finishing is diameter 30 ~ 40mm, and the spectrum bulk sample of height 30 ~ 40mm is numbered in the spectra sample marked;
(5) uniformity testing: from every group of spectral standard sample, choose 20 spectrum bulk samples arbitrarily, adopt direct reading spectrometry to carry out uniformity testing,, each element is carried out the homogeneity statistics according to analysis of variance;
(6) analyze definite value:
After the uniformity testing statistics is qualified; Car is got bits shape sample; Entrust the common also definite value of analyzing in the authoritative laboratory of domestic 8-10 family; Adopt the check of normal state method of inspection whether to be normal distribution to the definite value analytical data, adopt the check of Grubbs method whether to have outlier, each element is calculated its MV and standard deviation.
In such scheme, proportioning raw materials reasonable in design draws following sample.
Sample one: the chemical element that evenly contains following weight per-cent: Ni:14.96 ± 0.07%, C:2.50 ± 0.02%, Si:1.04 ± 0.02%, P:0.020 ± 0.001%; S:0.28 ± 0.01%, Co:0.98 ± 0.01%, Cu:0.12 ± 0.01%, Cr:1.94 ± 0.02%, Fe:77.85 ± 0.09%, surplus is an impurity.
Sample two: the chemical element that evenly contains following weight per-cent: Ni:18.62 ± 0.04%, C:1.02 ± 0.01%, Si:0.39 ± 0.01%, P:0.0325 ± 0.0005%; S:0.113 ± 0.006%, Co:0.60 ± 0.01%, Cu:0.049 ± 0.001%, Cr:1.49 ± 0.02%, Fe:77.66 ± 0.05%, surplus is an impurity.
Sample three: the chemical element that evenly contains following weight per-cent: Ni:25.95 ± 0.08%, C:1.45 ± 0.01%, Si:0.22 ± 0.01%, P:0.011 ± 0.001%; S:0.049 ± 0.002%, Co:0.46 ± 0.01%, Cu:0.015 ± 0.001%, Cr:1.08 ± 0.02%, Fe:70.74 ± 0.12%, surplus is an impurity.
Sample four: the chemical element that evenly contains following weight per-cent: Ni:30.77 ± 0.11%, C:0.47 ± 0.01%, Si:1.64 ± 0.01%, P:0.0060 ± 0.0008%; S:0.013 ± 0.001%, Co:1.27 ± 0.02%, Cu:0.14 ± 0.01%, Cr:0.72 ± 0.01%, Fe:64.66 ± 0.10%, surplus is an impurity.
Sample five: the chemical element that evenly contains following weight per-cent: Ni:40.54 ± 0.07%, C:0.096 ± 0.002%, Si:3.33 ± 0.01%, P:0.0092 ± 0.0002%; S:0.0095 ± 0.0004%, Co:1.87 ± 0.02%, Cu:0.19 ± 0.01%, Cr:0.36 ± 0.01%, Fe:52.77 ± 0.09%, surplus is an impurity.
Sample six: the chemical element that evenly contains following weight per-cent: Ni:49.07 ± 0.06%, C:0.036 ± 0.001%, Si:4.49 ± 0.02%, P:0.0042 ± 0.0005%; S:0.0020 ± 0.0002%, Co:2.01 ± 0.02%, Cu:0.25 ± 0.01%, Cr:0.13 ± 0.01%, Fe:42.74 ± 0.09%, surplus is an impurity.
Each chemical ingredients has rational gradient in the present invention's design; Be respectively 15 (± 1.5), 20 (± 1.5), 25 (± 1.5), 30 (± 1.5), 40 (± 1.5), 50 (± 1.5) like nickel; Other element also has distribution gradient like this, does not enumerate one by one at this.
Beneficial effect of the present invention: the present invention adopts direct pouring type casting as cast condition sample, solved can not forged standard model a preparation difficult problem; Sample interior weave construction uniformity, zero defect, chemical ingredients is even, sample good moldability, the rate of becoming a useful person height; For the high-carbon sample, need not add any modulator, can guarantee not have that graphite carbon is separated out, the sample whitening is good, avoided influence to sample composition and mensuration.
Achievement of the present invention can be applicable to high-carbon as cast condition and preparation that can not forged standard model, as conversion pig, foundry iron, can not forged other pig iron, ferronickel among high carbon steel and the present invention etc., range of application and field are wide.
Embodiment
Embodiment 1: the ferronickel spectral standard sample
The chemical element that evenly contains following weight per-cent: Ni:14.96 ± 0.07%, C:2.50 ± 0.02%, Si:1.04 ± 0.02%, P:0.020 ± 0.001%; S:0.28 ± 0.01%, Co:0.98 ± 0.01%, Cu:0.12 ± 0.01%, Cr:1.94 ± 0.02%, Fe:77.85 ± 0.09%, surplus is an impurity.
Embodiment 2: the ferronickel spectral standard sample
The chemical element that evenly contains following weight per-cent: Ni:18.62 ± 0.04%, C:1.02 ± 0.01%, Si:0.39 ± 0.01%, P:0.0325 ± 0.0005%; S:0.113 ± 0.006%, Co:0.60 ± 0.01%, Cu:0.049 ± 0.001%, Cr:1.49 ± 0.02%, Fe:77.66 ± 0.05%, surplus is an impurity.
Embodiment 3: the ferronickel spectral standard sample
The chemical element that evenly contains following weight per-cent: Ni:25.95 ± 0.08%, C:1.45 ± 0.01%, Si:0.22 ± 0.01%, P:0.011 ± 0.001%; S:0.049 ± 0.002%, Co:0.46 ± 0.01%, Cu:0.015 ± 0.001%, Cr:1.08 ± 0.02%, Fe:70.74 ± 0.12%, surplus is an impurity.
Embodiment 4: the ferronickel spectral standard sample
The chemical element that evenly contains following weight per-cent: Ni:30.77 ± 0.11%, C:0.47 ± 0.01%, Si:1.64 ± 0.01%, P:0.0060 ± 0.0008%; S:0.013 ± 0.001%, Co:1.27 ± 0.02%, Cu:0.14 ± 0.01%, Cr:0.72 ± 0.01%, Fe:64.66 ± 0.10%, surplus is an impurity.
Embodiment 5: the ferronickel spectral standard sample
The chemical element that evenly contains following weight per-cent: Ni:40.54 ± 0.07%, C:0.096 ± 0.002%, Si:3.33 ± 0.01%, P:0.0092 ± 0.0002%; S:0.0095 ± 0.0004%, Co:1.87 ± 0.02%, Cu:0.19 ± 0.01%, Cr:0.36 ± 0.01%, Fe:52.77 ± 0.09%, surplus is an impurity.
Embodiment 6: the ferronickel spectral standard sample
The chemical element that evenly contains following weight per-cent: Ni:49.07 ± 0.06%, C:0.036 ± 0.001%, Si:4.49 ± 0.02%, P:0.0042 ± 0.0005%; S:0.0020 ± 0.0002%, Co:2.01 ± 0.02%, Cu:0.25 ± 0.01%, Cr:0.13 ± 0.01%, Fe:42.74 ± 0.09%, surplus is an impurity.
Embodiment 7: the preparation method of ferronickel spectral standard sample
(1) raw material being added intermediate frequency furnace smelts:
Choose metallic nickel, high purity ferrosilicon (trade mark FeSi75-A), steel-making, is prepared burden by each constituent content of ferronickel spectral standard sample as raw material with the pig iron (trade mark L08), carbon steel (Q235), pure iron as raw material (trade mark YT01), chromium metal, metallic copper, cobalt metal, metallic aluminium, ferrophosphorus (trade mark FeP21), slag making materials fluorite, lime;
(2) adopt the formula cast that drenches with rain, the casting of water-cooled copper mould:
Gating system all adopts the pyroceramic goods, adopts the top mode that drenches with rain, and is even for guaranteeing composition, guarantees that no graphite carbon separates out, and adopts that copper mould is processed, manufacturing, water-cooled;
(3) adopt the tundish bottom pouring:
Molten steel changes tundish over to, and calm 10 minutes, open to water after 10 seconds and open water-in, water to finish and close water-in after 10 minutes, be incubated 45 minutes and take out standard sample for spectrochemical analysis;
(4) reconditioning, finishing and numbering:
With sample reconditioning and finishing is diameter 30 ~ 40mm, and the spectrum bulk sample of height 30 ~ 40mm is numbered in the spectra sample marked;
(5) uniformity testing:
The uniformity testing process is following:
Totally 6 groups of this cover spectral standard samples are chosen 20 spectrum bulk samples arbitrarily from every group of sample, adopt the direct reading spectrometry method that each element is carried out uniformity testing.According to analysis of variance, carry out homogeneity statistics: when statistic F ﹤ F α, then data do not have significant difference in the group and between group, and uniformity testing is qualified; When statistic F ﹥ F α, then the group in and the group between data there were significant differences, uniformity testing is defective.The uniformity testing data are seen table 1 ~ table 6.
Table 1 embodiment 1 uniformity testing data
Table 2 embodiment 2 uniformity testing data
Table 3 embodiment 3 uniformity testing data
Table 4 embodiment 4 uniformity testing data
Table 5 embodiment 5 uniformity testing data
Table 6 embodiment 6 uniformity testing data
Conclusion: through variance analysis legally constituted authority meter, each element statistic F value is all less than F
0.05(1.85), show that each element of this spectral standard sample has good uniformity.
(6) analyze definite value:
After the uniformity testing statistics was qualified, car was got bits shape sample, entrusted the common also definite value of analyzing in the authoritative laboratory of domestic 8-10 family.Adopt the check of normal state method of inspection whether to be normal distribution to the definite value analytical data, adopt the check of Grubbs method whether to have outlier.Each element is calculated its MV and standard deviation, see table 7.
Table 7 is analyzed the value data table
Claims (8)
1. ferronickel spectral standard sample, it is characterized in that: it evenly contains the chemical element of following weight per-cent:
Ni：14.9～50.0%；
C：0.03～2.50%；
Si：0.2～4.5%；
P：0.004～0.040%；
S：0.002～0.300%；
Co：0.4～2.0%；
Cu：0.01～0.25%；
Cr：0.1～2.0%；
Fe：40~80%；
Surplus is an impurity.
2. ferronickel spectral standard sample according to claim 1 is characterized in that: the chemical element that evenly contains following weight per-cent: Ni:14.96 ± 0.07%, C:2.50 ± 0.02%, Si:1.04 ± 0.02%, P:0.020 ± 0.001%; S:0.28 ± 0.01%, Co:0.98 ± 0.01%, Cu:0.12 ± 0.01%, Cr:1.94 ± 0.02%, Fe:77.85 ± 0.09%, surplus is an impurity.
3. ferronickel spectral standard sample according to claim 1 is characterized in that: the chemical element that evenly contains following weight per-cent: Ni:18.62 ± 0.04%, C:1.02 ± 0.01%, Si:0.39 ± 0.01%, P:0.0325 ± 0.0005%; S:0.113 ± 0.006%, Co:0.60 ± 0.01%, Cu:0.049 ± 0.001%, Cr:1.49 ± 0.02%, Fe:77.66 ± 0.05%, surplus is an impurity.
4. ferronickel spectral standard sample according to claim 1 is characterized in that: the chemical element that evenly contains following weight per-cent: Ni:25.95 ± 0.08%, C:1.45 ± 0.01%, Si:0.22 ± 0.01%, P:0.011 ± 0.001%; S:0.049 ± 0.002%, Co:0.46 ± 0.01%, Cu:0.015 ± 0.001%, Cr:1.08 ± 0.02%, Fe:70.74 ± 0.12%, surplus is an impurity.
5. ferronickel spectral standard sample according to claim 1 is characterized in that: the chemical element that evenly contains following weight per-cent: Ni:30.77 ± 0.11%, C:0.47 ± 0.01%, Si:1.64 ± 0.01%, P:0.0060 ± 0.0008%; S:0.013 ± 0.001%, Co:1.27 ± 0.02%, Cu:0.14 ± 0.01%, Cr:0.72 ± 0.01%, Fe:64.66 ± 0.10%, surplus is an impurity.
6. ferronickel spectral standard sample according to claim 1 is characterized in that: the chemical element that evenly contains following weight per-cent: Ni:40.54 ± 0.07%, C:0.096 ± 0.002%, Si:3.33 ± 0.01%, P:0.0092 ± 0.0002%; S:0.0095 ± 0.0004%, Co:1.87 ± 0.02%, Cu:0.19 ± 0.01%, Cr:0.36 ± 0.01%, Fe:52.77 ± 0.09%, surplus is an impurity.
7. ferronickel spectral standard sample according to claim 1 is characterized in that: the chemical element that evenly contains following weight per-cent: Ni:49.07 ± 0.06%, C:0.036 ± 0.001%, Si:4.49 ± 0.02%, P:0.0042 ± 0.0005%; S:0.0020 ± 0.0002%, Co:2.01 ± 0.02%, Cu:0.25 ± 0.01%, Cr:0.13 ± 0.01%, Fe:42.74 ± 0.09%, surplus is an impurity.
8. the preparation method of each described ferronickel spectral standard sample of claim 1 ~ 7 is characterized in that: may further comprise the steps:
(1) raw material being added intermediate frequency furnace smelts: adopt metallic nickel, ferrosilicon, the pig iron, carbon steel, pure iron, chromium metal, metallic copper, cobalt metal, metallic aluminium, ferrophosphorus, fluorite, lime as raw material, prepare burden by each constituent content of ferronickel spectral standard sample;
(2) adopt the formula cast that drenches with rain, the casting of water-cooled copper mould: gating system all adopts the pyroceramic goods, adopts the top mode that drenches with rain, and is even for guaranteeing composition, guarantees that no graphite carbon separates out, and adopts that copper mould is processed, manufacturing, water-cooled;
(3) adopt the tundish bottom pouring: molten steel changes tundish over to, and calm 10 minutes, open to water after 10 seconds and open water-in, water to finish and close water-in after 10 minutes, be incubated 45 minutes and take out standard sample for spectrochemical analysis;
(4) reconditioning, finishing and numbering: with sample reconditioning and finishing is diameter 30 ~ 40mm, and the spectrum bulk sample of height 30 ~ 40mm is numbered in the spectra sample marked;
(5) uniformity testing: from every group of spectral standard sample, choose 20 spectrum bulk samples arbitrarily, adopt direct reading spectrometry to carry out uniformity testing,, each element is carried out the homogeneity statistics according to analysis of variance;
(6) analyze definite value: after the uniformity testing statistics is qualified; Car is got bits shape sample; Entrust the common also definite value of analyzing in the authoritative laboratory of domestic 8-10 family; Adopt the check of normal state method of inspection whether to be normal distribution to the definite value analytical data, adopt the check of Grubbs method whether to have outlier, each element is calculated its MV and standard deviation.
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| CN103424396A (en) * | 2013-07-11 | 2013-12-04 | 江苏联峰能源装备有限公司 | Method for quickly analyzing all elements in cast iron sample by using emission spectrums |
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| 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 |
| CN103424396A (en) * | 2013-07-11 | 2013-12-04 | 江苏联峰能源装备有限公司 | Method for quickly analyzing all elements in cast iron sample by using emission spectrums |
| CN107111305A (en) * | 2014-12-05 | 2017-08-29 | 赛峰飞机发动机公司 | The method of analysis manufacture part while based on to statistical indicator |
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| 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 |
| CN113533014A (en) * | 2021-06-11 | 2021-10-22 | 中国科学院金属研究所 | Preparation method of internal control standard sample for spectral analysis of cast superalloy |
| CN113533014B (en) * | 2021-06-11 | 2022-07-26 | 中国科学院金属研究所 | Preparation method of internal control standard sample for spectral analysis of cast superalloy |
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