Preparation method applicable to the analysis of small-sized steel specimens by direct-reading spectrometers

Abstract

The present invention discloses a preparation method suitable for direct-reading spectrometer analysis of small-size steel samples, steps: preparation facilities: bending test machine, universal testing machine, direct-reading spectrometer, cutting machine, grinding machine and cylindrical steel sample; the cylindrical steel sample is cut by a cutting machine to obtain a first-cut sample with a length of 300mm-400mm, and the sample is bent by a bending test machine to obtain a U-shaped sample; the sample is cut again by a cutting machine from the U-shaped opening end to obtain a secondary intercepted steel sample with a length of 20mm-30mm, and the two ends of the secondary intercepted sample are placed on the pressing plate of the universal testing machine up and down forging to obtain an upsetting steel sample; the upsetting steel sample is ground flat with a grinding machine until the surface is smooth and the lines are consistent, that is, it is suitable for direct-reading spectrometer analysis of small-size steel samples. The sample analysis repeatability and reproducibility of the preparation method of the present invention are good after sample preparation, which fully proves that the present invention is practical.

Description

Technical Field

[0001] The present invention belongs to the technical field of sample modification, and relates to a preparation method for small-sized steel specimens suitable for analysis by a direct-reading spectrometer. Background Art

[0002] The excitation stage hole diameter of the ARL-3460 direct-reading spectrometer is 15 mm. According to the provisions of the spark discharge atomic spectrometry GB / T 4336-2016 for the determination of multi-element contents in low-carbon steel and medium-low alloy steel, the excitation hole must be completely covered during sample testing to ensure good excitation effect and accurate experimental data. For specimens with a nominal diameter of Φ10 mm - Φ16 mm, after vertical cutting and upsetting with a testing machine, they can be directly analyzed by the direct-reading spectrometer. For specimens with a nominal diameter of Φ6 mm - Φ8 mm, due to their too small diameter, the diameter after upsetting cannot reach more than 15 mm. We bought a sliding blade excitation stage, that is, there are two sliding blades with different excitation ports on the excitation stage, one with a diameter of 15 mm and the other with a diameter of 6.5 mm. Generally, the 15-mm sliding blade is used during the production process, and the 6.5-mm sliding blade is used for the component analysis of small-sized steel. However, the cross-sectional area of the steel with a diameter of Φ5.5 mm - Φ6.5 mm cannot completely and effectively cover the 6.5-mm excitation port, and the sample is too small to be well upset on the testing machine. How to meet the testing requirements of the ARL-3460 direct-reading spectrometer and ensure accurate and reliable test results has been studied by us. Summary of the Invention

[0003] The purpose of the present invention is to provide a preparation method for small-sized steel specimens suitable for analysis by a direct-reading spectrometer, which solves the problem in the prior art that the ARL-3460 direct-reading spectrometer cannot test specimens with a nominal diameter of Φ5.5 mm - Φ6.5 mm.

[0004] The technical solution adopted by the present invention is a preparation method for small-sized steel specimens suitable for analysis by a direct-reading spectrometer, which is specifically implemented according to the following steps:

[0005] Step 1, Prepare facilities: LWS-160 bending testing machine, WAW-300 electro-hydraulic servo universal testing machine, ARL-3460 direct-reading spectrometer, cutting machine, grinding machine, and cylindrical steel specimens;

[0006] Step 2, Cut the cylindrical steel specimens with a cutting machine to obtain a first-cut steel specimen with a length of 300 mm - 400 mm, bend the first-cut steel specimen with the LWS-160 bending testing machine to obtain a U-shaped bent steel specimen, and after bending, use the loading function to make the two ends of the obtained U-shaped bent steel specimen closely abut against each other to obtain a bent steel specimen;

[0007] Step 3, the bent steel sample is cut again from the U-shaped opening end with a cutting machine to obtain a secondary intercepted steel sample with a length of 20mm-30mm, and the two ends of the secondary intercepted steel sample are placed up and down on the pressing plate of the WAW-300 electro-hydraulic servo universal testing machine for upsetting to obtain an upsetting steel sample;

[0008] Step 4: Use a sample grinder to grind the end face of the top forged steel sample until the surface is smooth and flat with uniform texture, thus obtaining a small-sized steel sample suitable for analysis by a direct-reading spectrometer.

[0009] The present invention is also characterized in that:

[0010] The nominal diameter of the cylindrical steel specimen in step 1 is Φ5.5mm-Φ6.5mm.

[0011] The bending core during bending in step 2 is specifically 5mm-7mm.

[0012] In step 3, the two ends are placed up and down on the pressing plate, and the specific total height of the two ends is 11mm-13mm.

[0013] The specific upsetting in step 3 is:

[0014] Adjust the initial control speed of the pressure plate to 100N / s-300N / s, the final control force to 400N-600N, the initial control displacement to 10mm / min-30mm / min, and the final control displacement to 1 / 2-2 / 3 of the height of the steel sample;

[0015] During upsetting, the protective door is closed and the secondary cut steel sample is upset to 7mm-9mm.

[0016] The beneficial effects of the present invention are as follows: the present invention is applicable to the preparation method of small-sized steel samples for analysis by direct-reading spectrometer, the sample analysis data after sample preparation has good relative repeatability, and the reproducibility compared with the original molten steel results is also good, which fully proves that the present invention is applicable to the preparation method of small-sized steel samples for analysis by direct-reading spectrometer and has strong practicality. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a front view of a sample with a length of 15 mm cut off and bent in a preparation method for analyzing a small-size steel sample by a direct-reading spectrometer of the present invention;

[0018] Figure 2 It is a front view of a method for preparing a small-size steel sample for analysis by a direct-reading spectrometer according to the present invention, after the sample is upset on a testing machine and has a height of 2 / 3 of the original height;

[0019] Figure 3 It is a top view of a small-size steel sample after upsetting on a testing machine in a preparation method of the present invention suitable for analyzing a small-size steel sample by a direct-reading spectrometer. DETAILED DESCRIPTION

[0020] The present invention is described in detail below with reference to the accompanying drawings and specific embodiments.

[0021] The present invention is applicable to the preparation method of analyzing small-size steel samples by direct-reading spectrometer, and the specific operation steps are as follows:

[0022] Step 1. Prepare the equipment: LWS-160 bending test machine, WAW-300 electro-hydraulic servo universal testing machine, ARL-3460 direct reading spectrometer, cutting machine, grinding machine and cylindrical steel specimens;

[0023] The nominal diameter of the cylindrical steel sample in step 1 is Φ5.5mm-Φ6.5mm;

[0024] Step 2, cutting the cylindrical steel sample with a cutting machine to obtain a once-cut steel sample with a length of 300mm-400mm, bending the once-cut steel sample with an LWS-160 bending tester to obtain a U-shaped bent steel sample, and after bending, using a loading function to make the two ends of the U-shaped bent steel sample completely close to each other to obtain a bent steel sample;

[0025] The bending core during bending in step 2 is specifically 5mm-7mm;

[0026] Step 3, the bent steel sample is cut again from the U-shaped opening end with a cutting machine to obtain a secondary intercepted steel sample with a length of 20mm-30mm, and the two ends of the secondary intercepted steel sample are placed up and down on the pressing plate of the WAW-300 electro-hydraulic servo universal testing machine for upsetting to obtain an upsetting steel sample;

[0027] In step 3, the two ends are placed up and down on the pressing plate, and the total height of the two ends is 11mm-13mm;

[0028] The specific upsetting in step 3 is:

[0029] Adjust the initial control speed of the pressure plate to 100N / s-300N / s, the final control force to 400N-600N, the initial control displacement to 10mm / min-30mm / min, and the final control displacement to 1 / 2-2 / 3 of the height of the steel sample;

[0030] During upsetting, close the protective door and upset the secondary cut steel sample to 7mm-9mm;

[0031] Step 4: Use a sample grinder to grind the end face of the top forged steel sample until the surface is smooth and flat with uniform texture, thus obtaining a small-sized steel sample suitable for analysis by a direct-reading spectrometer.

[0032] Example 1

[0033] Step 1. Prepare the equipment: LWS-160 bending test machine, WAW-300 electro-hydraulic servo universal testing machine, ARL-3460 direct reading spectrometer, cutting machine, grinding machine and cylindrical steel specimens;

[0034] The nominal diameter of the cylindrical steel specimen in step 1 is Φ5.5 mm;

[0035] Step 2, cutting the cylindrical steel sample with a cutting machine to obtain a once-cut steel sample with a length of 300 mm, bending the once-cut steel sample with an LWS-160 bending tester to obtain a U-shaped bent steel sample, and after bending, using a loading function to make the two ends of the U-shaped bent steel sample completely close to each other to obtain a bent steel sample;

[0036] The bending core during bending in step 2 is specifically 5 mm;

[0037] Step 3, the bent steel sample is cut again from the U-shaped opening end with a cutting machine to obtain a secondary cut steel sample with a length of 20 mm, and the two ends of the secondary cut steel sample are placed up and down on the pressing plate of the WAW-300 electro-hydraulic servo universal testing machine for upsetting to obtain an upsetting steel sample;

[0038] In step 3, the two ends are placed up and down on the pressing plate, and the total height of the two ends is 11 mm;

[0039] The specific upsetting in step 3 is:

[0040] Adjust the initial control speed of the pressure plate to 100N / s, the final control force to 400N, the initial control displacement to 10mm / min, and the final control displacement to 1 / 2 of the height of the steel sample;

[0041] During upsetting, the protective door is closed and the secondary cut steel sample is upset to 7mm;

[0042] Step 4: Use a sample grinder to grind the end face of the top forged steel sample until the surface is smooth and flat with uniform texture, thus obtaining a small-sized steel sample suitable for analysis by a direct-reading spectrometer.

[0043] Example 2

[0044] Step 1. Prepare the equipment: LWS-160 bending test machine, WAW-300 electro-hydraulic servo universal testing machine, ARL-3460 direct reading spectrometer, cutting machine, grinding machine and cylindrical steel specimens;

[0045] The nominal diameter of the cylindrical steel specimen in step 1 is Φ6mm;

[0046] Step 2: Cut the cylindrical steel sample with a cutting machine to obtain a 350 mm long cut steel sample, bend the cut steel sample with a LWS-160 bending tester to obtain a U-shaped bent steel sample, and use a loading function after bending to make the two ends of the U-shaped bent steel sample completely close to obtain a bent steel sample;

[0047] The bending core during bending in step 2 is specifically 6 mm;

[0048] Step 3, the bent steel sample is cut again from the U-shaped opening end with a cutting machine to obtain a secondary cut steel sample with a length of 25 mm, and the two ends of the secondary cut steel sample are placed up and down on the pressing plate of the WAW-300 electro-hydraulic servo universal testing machine for upsetting to obtain an upsetting steel sample;

[0049] In step 3, the two ends are placed up and down on the pressing plate, and the total height of the two ends is 12 mm;

[0050] The specific upsetting in step 3 is:

[0051] Adjust the initial control speed of the pressure plate to 200N / s, the final control force to 500N, the initial control displacement to 20mm / min, and the final control displacement to 7 / 12 of the height of the steel sample;

[0052] During upsetting, the protective door is closed and the secondary cut steel sample is upset to 8mm;

[0053] Step 4: Use a grinding machine to grind the end face of the top forged steel sample until the surface is smooth and flat with uniform texture, thus obtaining a small-sized steel sample suitable for analysis by direct-reading spectrometer.

[0054] Example 3

[0055] Step 1. Prepare the equipment: LWS-160 bending test machine, WAW-300 electro-hydraulic servo universal testing machine, ARL-3460 direct reading spectrometer, cutting machine, grinding machine and cylindrical steel specimens;

[0056] The nominal diameter of the cylindrical steel specimen in step 1 is Φ6.5 mm;

[0057] Step 2: Cut the cylindrical steel sample with a cutting machine to obtain a once-cut steel sample with a length of 400 mm, bend the once-cut steel sample with an LWS-160 bending tester to obtain a U-shaped bent steel sample, and after bending, use a loading function to make the two ends of the U-shaped bent steel sample completely close to each other to obtain a bent steel sample;

[0058] The bending core during bending in step 2 is specifically 7 mm;

[0059] Step 3, the bent steel sample is cut again from the U-shaped opening end with a cutting machine to obtain a secondary cut steel sample with a length of 30 mm, and the two ends of the secondary cut steel sample are placed up and down on the pressing plate of the WAW-300 electro-hydraulic servo universal testing machine for upsetting to obtain an upsetting steel sample;

[0060] In step 3, the two ends are placed up and down on the pressing plate, and the total height of the two ends is 13mm;

[0061] The specific upsetting in step 3 is:

[0062] Adjust the initial control speed of the pressure plate to 300N / s, the final control force to 600N, the initial control displacement to 30mm / min, and the final control displacement to 2 / 3 of the height of the steel sample;

[0063] During upsetting, the protective door is closed and the secondary cut steel sample is upset to 9mm;

[0064] Step 4: Use a sample grinder to grind the end face of the top forged steel sample until the surface is smooth and flat with uniform texture, thus obtaining a small-sized steel sample suitable for analysis by a direct-reading spectrometer.

[0065] 1. Use the standard sample to verify that the equipment is in good condition. Punch 5 points on one surface. The results are as follows:

[0066] Slide excitation stage

[0067] Number C Si Mn S P V Standard sample 0.25 0.334 1.35 0.022 0.033 0.040 1 0.244 0.350 1.364 0.0231 0.0322 0.0411 2 0.251 0.341 1.355 0.0223 0.0331 0.0398 3 0.246 0.335 1.352 0.0225 0.0338 0.0399 4 0.243 0.336 1.339 0.0230 0.0339 0.0412 5 0.250 0.340 1.365 0.0241 0.0340 0.0409 Average value 0.247 0.340 1.355 0.0230 0.0334 0.041 Deviation -0.0032 0.0064 0.0050 0.0010 0.0004 0.0006 Allowable deviation ±0.02 ±0.03 ±0.035 ±0.005 ±0.007 ±0.01

[0068] Judging from the above data results, the equipment status analysis data is scientific and reliable.

[0069] 2. The above examples 1, 2 and 3 respectively use steel samples of Φ5.5 mm, Φ6 mm and Φ6.5 mm. After the samples are prepared according to the method of the present invention, they are analyzed on an ARL-3460 direct reading spectrometer using a slide excitation table. The results are shown in the following table:

[0070] Table 1: Molten steel furnace number 12202929 racket sample composition:

[0071] Number C Si Mn S P 12202929-1 0.232 0.434 1.422 0.023 0.035 12202929-2 0.241 0.441 1.408 0.0229 0.0334 12202929-3 0.238 0.438 1.419 0.0235 0.0345 12202929-4 0.236 0.450 1.428 0.0233 0.0352 12202929-5 0.245 0.446 1.433 0.0224 0.0349 Average value 0.238 0.442 1.422 0.023 0.035

[0072] Molten steel furnace number 12202929 corresponds to Φ5.5 steel 220320878 batch composition:

[0073] Number C Si Mn S P Average value of 12202929 0.238 0.442 1.422 0.023 0.035 220320878-1 0.241 0.431 1.441 0.0226 0.0334 220320878-2 0.250 0.445 1.430 0.0234 0.0350 220320878-3 0.233 0.451 1.425 0.0244 0.0341 220320878-4 0.229 0.426 1.436 0.0228 0.0354 220320878-5 0.234 0.422 1.420 0.0221 0.0337 Average value 0.237 0.435 1.430 0.023 0.034 Deviation -0.001 -0.007 0.008 0.000 -0.001 Allowable deviation ±0.02 ±0.03 ±0.035 ±0.005 ±0.007

[0074] Table 2: Molten steel furnace number 22202022 racket sample composition:

[0075] Number C Si Mn S P 22202022-1 0.231 0.433 1.350 0.0270 0.0217 22202022-2 0.229 0.424 1.361 0.0250 0.0207 22202022-3 0.234 0.445 1.346 0.0248 0.0203 22202022-4 0.230 0.442 1.332 0.0251 0.0241 22202022-5 0.218 0.432 1.352 0.0264 0.0230 Average value 0.228 0.435 1.348 0.0257 0.0220

[0076] The composition of the φ6 steel corresponding to the molten steel furnace number 22202022, batch number 220136114:

[0077]

[0078]

[0079] Table 3: The composition of the racket sample corresponding to the molten steel furnace number 22202905:

[0080] Number C Si Mn S P 22202905-1 0.621 0.206 0.612 0.0031 0.0112 22202905-2 0.612 0.211 0.622 0.0041 0.0122 22202905-3 0.624 0.220 0.618 0.0029 0.0113 22202905-4 0.634 0.213 0.630 0.0035 0.0124 22202905-5 0.631 0.212 0.606 0.0031 0.0115 Average value 0.624 0.212 0.618 0.003 0.012

[0081] The composition of the φ6.5 steel corresponding to the molten steel furnace number 22202905, batch number 220320808

[0082]

[0083]

[0084] It can be seen from the above Tables 1, 2, and 3 that the samples prepared by the method for preparing small-sized steel sample for direct-reading spectrometer analysis according to the present invention are analyzed on an ARL-3460 direct-reading spectrometer through a slide excitation stage, and the analysis results are all within the allowable deviation range.

[0085] 3. Select a furnace of molten steel with furnace number 22202022, collect a racket sample to represent the composition of this furnace, analyze it after milling, and also punch 5 points on one surface. The results are as follows:

[0086] Slide excitation stage

[0087] Number C Si Mn S P 22202022 0.220 0.440 1.360 0.025 0.021 1 0.231 0.433 1.350 0.0270 0.0217 2 0.229 0.424 1.361 0.0250 0.0207 3 0.234 0.445 1.346 0.0248 0.0203 4 0.230 0.442 1.332 0.0251 0.0241 5 0.218 0.432 1.352 0.0264 0.0230 Average value 0.228 0.435 1.348 0.0257 0.0220 Deviation 0.0084 -0.0048 0.012 0.0007 0.0010 Allowable deviation ±0.02 ±0.03 ±0.035 ±0.005 ±0.007

[0088] Select this furnace of molten steel with furnace number 22202022, analyze it on a conventional excitation stage (excitation aperture 15 mm) after milling, and also punch 5 points on one surface. The results are as follows:

[0089] Conventional excitation stage

[0090] Number C Si Mn S P V 22202022 0.220 0.440 1.380 0.025 0.021 0.014 1 0.225 0.433 1.370 0.0244 0.0214 0.0130 2 0.233 0.442 1.400 0.0240 0.0233 0.0130 3 0.230 0.428 1.411 0.0252 0.0224 0.0140 4 0.234 0.436 1.420 0.0260 0.0220 0.0140 5 0.214 0.427 1.380 0.0239 0.0205 0.0130 Average value 0.227 0.433 1.396 0.0247 0.0219 0.0134 Deviation 0.007 -0.007 0.016 -0.0003 0.0009 -0.0006 Allowable deviation 0.02 0.03 0.035 0.005 0.007 0.01

[0091] To sum up: The sample analysis data after sample preparation by the method for preparing small-sized steel sample for direct-reading spectrometer analysis according to the present invention has relatively good repeatability, and also good reproducibility when compared with the results of the original molten steel, fully proving that the method for preparing small-sized steel sample for direct-reading spectrometer analysis according to the present invention has strong practicability.

Claims

1. Preparation method for small-size steel samples analyzed by direct reading spectrometer. It is characterized in that Follow the steps below to implement it: Step 1. Prepare the following equipment: LWS-160 bending test machine, WAW-300 electro-hydraulic servo universal testing machine, ARL-3460 direct reading spectrometer, cutting machine, grinding machine and cylindrical steel specimens. The nominal diameter of the cylindrical steel specimens is Φ5.5mm-Φ6.5mm. Step 2, cutting the cylindrical steel sample with the cutting machine to obtain a once-cut steel sample with a length of 300mm-400mm, bending the once-cut steel sample with an LWS-160 bending tester, with a bending core of 5mm-7mm during bending, to obtain a U-shaped bent steel sample, and after bending, using a loading function to make the two ends of the U-shaped bent steel sample completely close to each other, to obtain a bent steel sample; Step 3, the bent steel sample is cut again from the U-shaped opening end with a cutting machine to obtain a secondary intercepted steel sample with a length of 20mm-30mm, and the two ends of the secondary intercepted steel sample are placed up and down on the pressing plate of the WAW-300 electro-hydraulic servo universal testing machine for upsetting, and the total height of the two ends is 11mm-13mm. The upsetting is specifically as follows: the initial control speed of the pressing plate is adjusted to 100N / s-300N / s, the final control force is 400N-600N, the initial control displacement is 10mm / min-30mm / min, and the final control displacement is 1 / 2-2 / 3 of the height of the steel sample; the protective door is closed during upsetting, and the secondary intercepted steel sample is upset to 7mm-9mm to obtain an upset steel sample; Step 4: Grind the end surface of the top forged steel sample with a grinding machine until the surface is smooth and flat with uniform texture, thereby obtaining a small-sized steel sample suitable for analysis by a direct-reading spectrometer.

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