KR0159119B1 - Solution for measurement of steel macro structure and its measurement method - Google Patents
Solution for measurement of steel macro structure and its measurement method Download PDFInfo
- Publication number
- KR0159119B1 KR0159119B1 KR1019930030178A KR930030178A KR0159119B1 KR 0159119 B1 KR0159119 B1 KR 0159119B1 KR 1019930030178 A KR1019930030178 A KR 1019930030178A KR 930030178 A KR930030178 A KR 930030178A KR 0159119 B1 KR0159119 B1 KR 0159119B1
- Authority
- KR
- South Korea
- Prior art keywords
- solution
- measuring
- steel
- macrostructure
- surfactant
- Prior art date
Links
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 11
- 239000010959 steel Substances 0.000 title claims abstract description 11
- 238000005259 measurement Methods 0.000 title description 4
- 238000000691 measurement method Methods 0.000 title description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 8
- 238000005242 forging Methods 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000004040 coloring Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N2015/103—Particle shape
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
본 발명은 철강의 마크로 조직을 측정하는데 필요한 측정용 용액 및 측정하는 방법에 관한 것이다.The present invention relates to a measuring solution and a measuring method necessary for measuring the macrostructure of steel.
본 발명의 철강의 마크로 조직 측정용 용액은 증류수 80-120㎖, 피크린산3-5g, 계면활성제 3-5g, 염산 0.3-0.7㎖로 조성된 것을 특징으로 한다.The solution for measuring the macrostructure of steel of the present invention is characterized in that it is composed of distilled water 80-120ml, picric acid 3-5g, surfactant 3-5g, hydrochloric acid 0.3-0.7ml.
본 발명의 철강의 마크로 조직 측정방법은 증류수 80-120㎖, 피크린산3-5g, 계면활성제 3-5g, 염산 0.3-0.7㎖로 조성된 용액을 65-95℃정도의 온도로 가열 유지하는 단계와, 시험편을 상기 용액에 담근 후 2-5분 정도 유지시키는 단계와, 상기 시험편을 꺼내어 세척, 건조 후 측정하는 단계로 구성된다.The method for measuring the macrostructure of steel of the present invention comprises the steps of maintaining and maintaining a solution composed of distilled water 80-120ml, picric acid 3-5g, surfactant 3-5g, hydrochloric acid 0.3-0.7ml to a temperature of about 65-95 ℃ After immersing the test piece in the solution for 2-5 minutes, and taking out the test piece, washing, drying and measuring the steps.
Description
제1도는 시험 방법의 개략도.1 is a schematic representation of a test method.
제2도는 본 발명에 의한 현출된 철강의 마크로 조직 (2.5배).2 is a macrostructure (2.5 times) of manifested steel according to the present invention.
본 발명은 철강의 마크로 조직을 측정하는데 필요한 측정용 용액 및 측정하는 방법에 관한 것이다.The present invention relates to a measuring solution and a measuring method necessary for measuring the macrostructure of steel.
마크로 조직(Macro Structure)이란 육안 또는 확대경으로 결정의 분포상태, 형상, 크기 등에 대하여 관찰한 것으로서 화학조성, 조직의 균일도, 수지상정, 기포, 균열 등을 검출하는데 많이 사용되고 있다.Macro structure is an observation of the distribution, shape and size of crystals with the naked eye or a magnifying glass, and is widely used to detect chemical composition, uniformity of tissue, dendrite, bubbles, and cracks.
철강의 마크로 조직은 기계 구조용 소재의 가공정도 및 철강재의 압연, 단조, 열처리 등에 의해 각기 달리 형성되며 생성된 조직에 따라 각 소재의 성질에 많은 영향을 미친다. 이러한 마크로 조직에 대한 관찰은 소재의 이력 및 미세 조직과 연관하여 소재의 물성치 예측에 크게 기여 할 수 있으며 각종 소재의 성질, 방향성을 쉽게 측정 관찰 할 수 있다.The macro structure of steel is formed differently by the degree of processing of mechanical structural materials and the rolling, forging, and heat treatment of steel materials, and has a great influence on the properties of each material depending on the generated structure. Observation of the macro structure can greatly contribute to the prediction of material properties in relation to the history and microstructure of the material, and can easily measure and observe the properties and orientation of various materials.
종래 마크로 조직의 측정은 주로 ASTM(American Standards for Testing and Materials)과 JIS(Japanese Industrial Standard) 규격에 의거 행하여져 왔다.The measurement of conventional macrostructures has been carried out mainly in accordance with American Standards for Testing and Materials (ASTM) and Japanese Industrial Standard (JIS) standards.
ASTM에서는 염산 : 증류수의 비가 1:1인 용액을 추천하고 있으며, JISGO553의 강의 마크로 조직 시험 방법에서는 단련 철강품의 단조선(Metal Flow)관찰을 위해서 염산 20%수용액에서 75-80℃로 30분간 가열하는 방법을 추천하고 있다. 그러나 이 두가지 방법은 모두 단조선이 명확히 드러나지 않는다.ASTM recommends a solution with a ratio of hydrochloric acid: distilled water of 1: 1. For the macrostructure test method of JISGO553, heat is heated at 75-80 ℃ for 30 minutes in 20% aqueous hydrochloric acid solution to observe the metal flow of annealed steel products. I recommend the way. However, both of these methods do not clearly reveal the forging ship.
그 이유는 가열중 고농도의 HCl이 휘발함으로써 농도가 감소하는 것과, HCl이 침식하면서 탈색효과에 기인하여 심하게 부식되어도 부식 부위가 확실히 구분되지 않기 때문이다.The reason for this is that the concentration decreases due to the volatilization of high concentrations of HCl during heating, and the corrosion sites are not clearly distinguished even if HCl is eroded severely due to the decolorization effect.
상기 문제점을 해결하기 위하여 본 발명은 침식이 심하게 되지 않아 시편의 조직 검사등 다른 용도에 재사용이 가능하며 특히 단조선 부위에서는 선택적인 부식에 기인하여 육안으로도 쉽게 마크로 조직을 관찰할 수 있는 철강의 마크로 조직 측정용 용액 및 측정 방법을 제공한다.In order to solve the above problems, the present invention can be reused for other purposes such as inspection of specimens because the erosion is not severe. Especially, in the forging part, due to selective corrosion, it is possible to observe the macrostructure easily with the naked eye. A solution for measuring macrotissue and a measuring method are provided.
본 발명의 마크로 조직 측정용 용액은 증류수 80-120㎖, 피크린산3-5g, 계면활성제 3-5g, 염산 0.3-0.7㎖로 조성되며 계면활성제는 소디윰 벤젠 설파네이트(Sodium Dedecylbenzene sulfonate)인 것을 특징으로 한다.Macro-measurement solution of the present invention is composed of distilled water 80-120ml, picric acid 3-5g, surfactant 3-5g, hydrochloric acid 0.3-0.7ml and the surfactant is Sodium Dedecylbenzene sulfonate (Sodium Dedecylbenzene sulfonate) It is done.
또한 본 발명은 마크로 조직측정방법은 증류수 80-120㎖, 피크린산3-5g, 계면활성제 3-5g, 염산 0.3-0.7㎖로 조성된 용액을 65-95℃ 정도의 온도로 가열 유지하는 단계와, 시험편을 상기 용액에 담근 후 2-5분 정도 유지시키는 단계와, 상기 시험편을 꺼내어 세척 건조 후 측정하는 단계로 구성되는 것을 특징으로 한다.In addition, the present invention is a macrostructure measurement method is the step of maintaining the solution of distilled water 80-120ml, picric acid 3-5g, surfactant 3-5g, hydrochloric acid 0.3-0.7ml solution at a temperature of about 65-95 ℃, After immersing the test piece in the solution for 2 to 5 minutes, and taking out the test piece, characterized in that it comprises a step of measuring after washing and drying.
이하 상기 용액의 성분 조성 및 측정조건을 수치 한정하는 이유에 대하여 설명한다.Hereinafter, the reason for numerically limiting the component composition and the measurement conditions of the solution will be described.
피크린산은 가공에 의해 형성된 단조선(Metal Flow)을 착색시켜 마크로 조직을 가시화시키는 작용을 하며 3-5g 첨가하는 이유는 3g이하 첨가시에는 조직을 착색시키는 피크린산의 작용이 충분하지 못하여 명확한 마크로 조직을 관찰할 수 없으며 5g이상을 상기 용액에 첨가시에는 피크린산의 농도가 증가하여도 마크로 조직 착색에 큰 영향을 미치지 않으므로 피크린산의 농도 범위를 정하였다.Picric acid acts to visualize the macro structure by coloring the metal flow formed by processing, and the reason for adding 3-5g is that the action of picric acid coloring the tissue is not enough to add a clear macro structure. When 5 g or more was added to the solution, the concentration range of picric acid was determined since the concentration of picric acid did not have a significant effect on the coloration of macro tissues.
계면활성제는 피크린산의 침투를 돕는 역할을 하여 단조선 착색을 용이하게 한다. 3-5g 첨가하는 이유는 계면활성제의 특성상 물 100㎖당 3g이하에서는 활성제로서의 역할을 하지 못하며 또한 5g이상에서는 농도가 증가하여도 그 효과가 좋아지지 않는다. 따라서 계면활성제의 농도 범위를 설정하였다.Surfactants serve to aid in the penetration of picric acid to facilitate forging of the forging line. The reason for the addition of 3-5g is that due to the nature of the surfactant does not play a role as the active agent in less than 3g per 100ml of water, and the effect is not improved even if the concentration increases above 5g. Therefore, the concentration range of surfactant was set.
염산은 피검면에서 발생하는 산화막을 제거하고 또한 표면을 세척시키는 작용을 하여 계속적인 현출 작용이 이루어지도록 한다. 0.3-0.7㎖ 첨가하는 이유는 0.7㎖이상 첨가하였을 경우 시료 표면의 부식작용이 심하여 피크린산으로 착색시킨 조직이 녹게 되어 마크로 조직관찰이 어려워지며 0.3㎖ 이상으로 설정한 것은 세척작용을 확보하기 위한 것이다.Hydrochloric acid removes the oxide film generated from the surface to be inspected, and also cleans the surface, so that the continuous appearance is achieved. The reason for adding 0.3-0.7ml is that when 0.7ml or more is added, the corrosion of the sample surface is so severe that the tissues colored with picric acid are dissolved, making it difficult to observe the macrostructure.
용액을 65-95℃ 정도의 온도로 가열하는 이유는 65℃ 이하의 온도에서는 상기 조성의 용액으로도 상당히 장시간을 요하므로 65℃ 이상으로 정하였으며, 95℃ 이상의 온도는 물의 끓는 점으로 화학 성분이 비산하여 용액의 조성이 변화하기 때문이다.The reason for heating the solution to a temperature of about 65-95 ° C. was set at 65 ° C. or higher since the solution of the composition required a very long time at a temperature below 65 ° C., and the temperature above 95 ° C. was the boiling point of water. This is because the composition of the solution changes due to scattering.
시험편을 2-5분간 용액에 담그는 이유는 2분 이하의 시간에서는 충분한 부식반응이 발생하지 않아 조직관찰이 어려우며 5분 이상 담그는 조직의 변화는 없기 때문이다.The reason why the specimen is immersed in the solution for 2-5 minutes is that it will be difficult to observe the tissue because there is not enough corrosion reaction in less than 2 minutes.
이하의 실시예를 통해 본 발명을 설명한다.The present invention will be described through the following examples.
[실시예]EXAMPLE
증류수 80-120㎖, 피크린산 3-5g, 소디움 도데실벤젠 설파네이트 3-5g, 염산 0.3-0.7㎖로 조성된 용액을 파이랙스(Pylex)제품의 비이커에서 온도를 승온시켜 65-95℃ 정도로 유지시킨 후 시험편을 제1도와 같이 용액에 완전히 담근 후 2-5분 정도 유지시킨다. 그 후 시험편을 꺼내어 흐르는 증류수내에서 세척하고 탈지면을 사용하여 표면의 흑피층을 제거한 후 다시 세척, 건조 시킨 후 육안, 확대경 혹은 줌 카메라를 이요하여 관찰한다.A solution of 80-120 ml of distilled water, 3-5 g of picric acid, 3-5 g of sodium dodecylbenzene sulfonate, and 0.3-0.7 ml of hydrochloric acid was heated to a temperature of about 65-95 ° C. in a beaker of Pylex. After soaking the specimen completely in the solution as shown in Figure 1 and hold for 2-5 minutes. Then remove the specimen and wash it in running distilled water, remove the black layer on the surface using cotton wool, wash and dry again, and then observe it with a naked eye, a magnifying glass, or a zoom camera.
위와 같이 처리된 시험편은 제2도에 나타난 바와 같이 선명한 마크로 조직이 현출된다.As described above, the specimens treated as described above exhibited a clear mark structure as shown in FIG.
본 발명의 가장 큰 특징은 ASTM이나 JIS에서 추천하는 방법에 비해 처리시간이 약 1/10로 단축되며 또한 깨끗한 마크로 조직을 얻을 수 있다.The biggest feature of the present invention is that the processing time is shortened by about 1/10 compared to the method recommended by ASTM or JIS, and a clear macro structure can be obtained.
따라서 이에 대한 관찰도 현장이나 분석실에서 간단한 장비나 육안으로도 쉽게 관찰이 가능하며 표면 침식량이 많지 않아 시험편의 재사용이 용이하다. 따라서 기존의 방식에 비하여 처리시간이 단축되고 가열시 발생하는 염산증기의 양이 적어 작업시 안전하며 고품질의 마크로 조직을 쉽게 관찰할 수 있으며 사진촬영이 가능하여 관련된 재료의 품질 관리 효과면에서 중요한 기술을 제공할 수 있다.Therefore, this observation can be easily observed in the field or analysis room by simple equipment or the naked eye, and it is easy to reuse the test specimen because there is not much surface erosion amount. Therefore, the processing time is shortened compared to the existing method, and the amount of hydrochloric acid generated during heating is safe, so it is safe for work, high quality macro tissue can be easily observed, and photographing is possible, which is an important technology in terms of quality control effect of related materials. Can be provided.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019930030178A KR0159119B1 (en) | 1993-12-28 | 1993-12-28 | Solution for measurement of steel macro structure and its measurement method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019930030178A KR0159119B1 (en) | 1993-12-28 | 1993-12-28 | Solution for measurement of steel macro structure and its measurement method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR950019706A KR950019706A (en) | 1995-07-24 |
| KR0159119B1 true KR0159119B1 (en) | 1999-05-01 |
Family
ID=19373198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1019930030178A KR0159119B1 (en) | 1993-12-28 | 1993-12-28 | Solution for measurement of steel macro structure and its measurement method |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR0159119B1 (en) |
-
1993
- 1993-12-28 KR KR1019930030178A patent/KR0159119B1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| KR950019706A (en) | 1995-07-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Truman | The influence of chloride content, pH and temperature of test solution on the occurrence of stress corrosion cracking with austenitic stainless steel | |
| JPS6339674B2 (en) | ||
| CN109238813A (en) | The detection display methods of spring steel austenite grain | |
| CN107236955B (en) | A kind of metallographic etching agent and the metallographic phase display method for showing crackle microscopic structure | |
| CN113358646B (en) | Corrosive agent for testing 16MnCr5 steel austenite grain boundary and testing method thereof | |
| CN112048720A (en) | Nickel-based powder superalloy corrosion solution and corrosion method | |
| KR0159119B1 (en) | Solution for measurement of steel macro structure and its measurement method | |
| US20120000412A1 (en) | Method Of Colouring Tin And Tin-Containing Articles | |
| US3652225A (en) | Color method for detecting cracks in metal bodies | |
| CA1056702A (en) | Composition and method for cleaning aluminum at low temperatures | |
| US4383042A (en) | Process for detecting soft spots in aluminum | |
| KR20120097161A (en) | Etching solution for exposure of austenite grain size and method for exposure of austenite grain size using thereof | |
| US3652224A (en) | Method for detecting cracks in metal bodies | |
| SU1481267A1 (en) | Method of etching materials | |
| CN113340698B (en) | Eroding agent for observing metallographic structure of zirconium alloy and method for preparing metallographic sample of zirconium alloy | |
| US2959471A (en) | Acid etch inspection process | |
| KR0159120B1 (en) | Measurement solution for steel austement crystallization and measurement method thereof | |
| CN108300998A (en) | Show aggressive agent, the preparation method and application of P91 and P92 steel original austenite crystal preventions | |
| Pagel et al. | Effect of temperature on tributyl phosphate as extracting agent for organic acids | |
| CN106840822B (en) | A kind of surface treatment method measuring stainless oxygen content in steel sample | |
| Sheasby et al. | A Quantitative Method of Testing the Quality of Sealing of Anodized Aluminium | |
| US2839918A (en) | Flaw detection | |
| DE102018201668B4 (en) | Method for the non-destructive testing of workpiece surfaces | |
| CN109557107A (en) | A kind of method for detection fault detection of stainless steel/carbon composite material | |
| Onoro et al. | Stress corrosion cracking model in 7075 aluminium alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E701 | Decision to grant or registration of patent right | ||
| GRNT | Written decision to grant | ||
| LAPS | Lapse due to unpaid annual fee |