CN102305736A - Method for preparing leather sample observed by metallurgical microscope - Google Patents
Method for preparing leather sample observed by metallurgical microscope Download PDFInfo
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- CN102305736A CN102305736A CN201110179680A CN201110179680A CN102305736A CN 102305736 A CN102305736 A CN 102305736A CN 201110179680 A CN201110179680 A CN 201110179680A CN 201110179680 A CN201110179680 A CN 201110179680A CN 102305736 A CN102305736 A CN 102305736A
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Abstract
The invention relates to a method for preparing a leather sample observed by a metallurgical microscope, and belongs to the technical field of leather inspection. The method comprises the following steps of: (1) adding a promoter into an unsaturated polyester resin, stirring, adding a curing agent, stirring, standing, and discharging the mixed air to obtain an immobilized resin; (2) immersing a sample into the immobilized resin, and curing to obtain a cured sample; (3) grinding both ends of the cured sample until the ends are flat, fixing in a mould, injecting the immobilized resin into the mould, curing, demoulding, and post-curing to obtain a post-cured sample block; and (4) grinding and polishing the post-cured sample block by using abrasive paper to obtain the leather sample observed by the metallurgical microscope. In the method, the unsaturated polyester resin is used as a main ingredient of the immobilized resin, and operation steps are designed according to a capillary action principle to ensure that the immobilized resin can be quickly and fully permeated into the leather sample, so the adhesion and deformation of section fiber of leather are furthest avoided.
Description
Technical field
The present invention relates to a kind of preparation method of leather sample, be specifically related to a kind of leather sample preparation methods that is applicable to the metallography microscope sem observation, belong to leather inspection technology field.
Background technology
Leather quality is reflected by finished leather physical and chemical index and organoleptic properties index usually.The organoleptic indicator comprises: richness, pliability, elasticity, can't measure by instrument at present, and technician's hand is touched and is made evaluation soon by rule of thumb.Owing to it be unclear that the quantitative relationship between leather micromechanism and the finished leather macro property, watch and the rough judgement at the goods otch is controlled at Products Quality so can only artificial hand on the tanning production touch.
The leather institutional framework is the internal factor of decision finished leather performance, and it is meant the fibre morphology of leather collagen, can characterize with 3 indexs usually: uniformity coefficient, shatter value and angle of weave.Set up the mathematical model of leather institutional framework parameter and leather sense index and physical performance index, will scientific basis be provided for seeking the internal factor that influences leather sense organ and physical property; Help to instruct and control the leather fiber loosening degree aborning, finally reach purpose (exploration of mathematical model between leather microstructural parameter and the finished leather performance parameter, the Yang Yun of control leather quality; Chinese leather ISSN 1001-6813; The 35th the 13rd phase of volume, 19-21 page or leaf, in July, 2006).
Leather institutional framework parameter mainly obtains through observing the leather histotomy now, and as 2002, the Wang Yingmei of Sichuan University etc. carried out studying (sucking pig skin institutional framework research through the section of polarized light microscope observing sucking pig skin to sucking pig skin institutional framework; Wang Yingmei etc., leather science and engineering ISSN 1004-7964, the 12nd volume; The 1st phase, 50-54 page or leaf, in February, 2002); 2010, the Lv Jing of resource and environment institute of Shaanxi Tech Univ removed from office histotomy with pig, sheep, ox-hide finished product that sulfuric acid Nai Erlan decoration method has prepared different feels, observes its institutional framework at the multimedia microscopically; Relation (institutional framework of pig, sheep, ox-hide finished product leather and the relation discussion of performance, leather and chemical industry ISSN 1674-0939, the 27th volume of its institutional framework and performance have been analyzed; The 6th phase, 36-39 page or leaf, in Dec, 2010).
But, in the slice processing process, receiving the pressure of slicer, embedding medium can compress, and shrinkage appears in section thereupon, influences the optical microscopic image quality.In addition, fiber is intensive, crisscross in the leather, and thickness is uneven, in slicing processes, be easy to generate fiber crimp, come off or fiber between the glutinous phenomenon that connects, cause the leather sample fibre section distortion of section, be difficult to extract section feature parameter accurately.
Summary of the invention
The present invention is directed to the deficiency of prior art, provide a kind of and make that leather cross-section fibers distortion is little, edge contour is with internal feature is clear, can accurately reflect the leather institutional framework, the leather sample fast preparation method of suitable metallography microscope sem observation.
Summary of the invention
The present invention uses unsaturated polyester resin, promoter and curing agent mixture dipping leather sample; Be made into a kind of firm polymer matrix composites after the curing, leather fiber is fixed, can polish to it, operation such as polishing; And fiber is mobile, indeformable, does not lack.
Detailed Description Of The Invention
A kind of leather sample preparation methods that is applicable to the metallography microscope sem observation, step is following:
(1) elder generation adds the promoter of 0.5～2 mass parts in the unsaturated polyester resin of 100 mass parts, stirs 5～10 minutes, and then adds the hardening agent of 1～3 mass parts; Stirred 5～10 minutes, and then, left standstill 8～15 minutes; The air that discharge is sneaked into obtains fixing resin;
(2) sample is immersed in the fixing resin that step (1) makes, after fixing resin infiltrates sample fully, takes out sample, in 60 ℃ of thermostatic drying chambers, solidified 1～2 hour, solidified sample;
(3) the solidified sample two ends that step (2) made polish, and are fixed in the mould fixing resin that implantation step in mould (1) makes then; 25 ℃ solidified 1～2 hour, and the demoulding obtains the appearance piece that the middle part is fixed with solidified sample; Solidified after 60 ℃ 1～2 hour, and got the back and solidify an appearance piece;
(4) the back curing appearance piece that step (3) is made makes the leather sample that is applicable to the metallography microscope sem observation after sand papering, polishing.
Unsaturated polyester resin in the said step (1) be fiberglass with adjacent benzene/metaphenylene unsaturated polyester resin or vinyl esters unsaturated polyester resin, promoter is cobalt iso-octoate or cobalt naphthenate, hardening agent is methyl ethyl ketone peroxide or cyclohexanone peroxide.
Adopt following method to make fixing resin infiltrate sample fully in the said step (2):
With the fixing resin that sample one end in contact step (1) makes, keep sample to stand on the fixing resin top then, left standstill 0.5～2 hour, fixing resin gets into interfibrous space in the sample, and the complete filling space, gets final product.This step utilizes the small spaces between leather fiber can produce capillary action to resin, and resin is sucked interfibrous space fully, thereby bubble can't be discharged and the cavitation that causes between the fiber of having avoided being caused by immersion.
Sample in the said step (2) is the leather bar of long 15～25mm, wide 1.5～2.5mm.
Mould in the said step (3) is the cylindrical mold of internal diameter 30～50mm, high 15-25mm.
Sand papering in the said step (4) is for use 200 orders, 320 orders, 500 orders, 1000 orders, 1500 orders, 2000 orders, 3000 order liquid honings successively.
150～300 rev/mins of metallurgical polishing machines that are finished in the said step (4) polished 1～2 minute.
Beneficial effect
Preparation method of the present invention, owing to adopt the principal ingredient of unsaturated polyester resin as fixing resin, simultaneously according to capillary action principle design operation steps; Fixing resin can be infiltrated in the leather sample fast, fully; In addition, adopt capillary action can the air in the leather pore be discharged, suck fixing resin fully; Keep original attitude of leather fiber, avoided the deformation in leather fiber cross section to greatest extent.Fixing resin and leather fiber be nature difference very big two mutually, in metaloscope, can observe edge contour and internal feature clearly, thereby accurately reflect the leather institutional framework.
Description of drawings
Fig. 1 is the synoptic diagram of structures of samples described in the embodiment;
Fig. 2 is the structural representation that solidifies the appearance piece described in the embodiment;
Fig. 3 is the photo that the sample in cross section of embodiment 1 shows in the metaloscope eyepiece;
Fig. 4 is the photo that the sample in cross section of embodiment 2 shows in the metaloscope eyepiece;
Fig. 5 removes from office the institutional framework photo through the section that gelatin immersion, formaldehyde fixed, sulfuric acid Nai Erlan dye liquor decoration method make at the observable ox-hide finished product of multimedia microscopically;
Fig. 6 is through the blue leather of the observable pigskin of routine paraffin wax embedded section institutional framework photo.
Embodiment
Below in conjunction with embodiment and Figure of description, the present invention is done further elaboration, but institute of the present invention protection domain is not limited thereto.
The unsaturated polyester resin of 196# described in the embodiment, 191# unsaturated polyester resin, 50% cobalt iso-octoate solution (every microlitre contains 0.40～0.45 milligram of cobalt iso-octoate), 50% methyl ethyl ketone peroxide solution (every microlitre contains 0.54～0.60 milligram of methyl ethyl ketone peroxide, contains available oxygen≤10%), cobalt naphthenate, cyclohexanone peroxide are all available from Jinan resin glass fibre reinforced plastics technology development center.
A kind of leather sample preparation methods that is applicable to the metallography microscope sem observation, step is following:
(1) earlier 350ul 50% cobalt iso-octoate solution is added in the 70g 196# unsaturated polyester resin, stir 5 minutes; And then add 700ul 50% methyl ethyl ketone peroxide solution, stirred 10 minutes, then; Left standstill 10 minutes, and discharged the air of sneaking into, obtain fixing resin;
(2) sample of ox-hide that drying is good leather cutting growth 20mm, wide 2mm with the fixing resin that sample one end in contact step (1) makes, keeps sample to stand on the fixing resin top then; Left standstill 1.5 hours; Fixing resin gets into interfibrous space in the sample, and the complete filling space, takes out sample; In 60 ℃ of thermostatic drying chambers, solidified 2 hours, get solidified sample;
(3) the solidified sample two ends that step (2) made polish, and a end is fixed in the bottom centre position of the cylindrical mold of internal diameter 40mm, high 20mm then, makes sample stand upright on mould central authorities; The fixing resin that implantation step in mould (1) makes; 25 ℃ solidified 2 hours, and the demoulding obtains the appearance piece that the middle part is fixed with solidified sample; Solidified 1 hour after 60 ℃, get the back and solidify an appearance piece;
(4) the back curing appearance piece that step (3) is made after 2 minutes, makes the leather sample that is applicable to the metallography microscope sem observation through 200 orders, 320 orders, 500 orders, 1000 orders, 1500 orders, 2000 orders, 3000 order liquid honings, 300 rev/mins of metallurgical polishing machine polishings successively.
Through the metallography microscope sem observation, the result is as shown in Figure 3.
Utilize the method in " institutional framework of pig, sheep, ox-hide finished product leather and the relation of performance are inquired into " literary composition in the background technology; With aqueous gelatin solution soak, formalin fixedly is unstained and cuts into slices behind the ox-hide finished product leather kind piece; Section is broken up with glacial acetic acid after being dipped in the dyeing of sulfuric acid Nai Erlan dye liquor again, uses the Arabic gum sealing at last.Observe this sample section at the multimedia microscopically, the institutional framework photo that obtains ox-hide finished product leather is as shown in Figure 5.
Fig. 5 compares with Fig. 3, and fiber does not have adhesion among visible Fig. 3, does not have distortion, and profile is more clear, more helps observing.
Embodiment 2
Like embodiment 1 described preparation method, difference is that unsaturated polyester resin is the 191# unsaturated polyester resin, and consumption is 80g; Promoter is cobalt naphthenate, and consumption is 800ul; Hardening agent is a cyclohexanone peroxide, and consumption is 1200ul.
Through the metallography microscope sem observation, the result is as shown in Figure 4.
As shown in Figure 6 through the blue leather of the observable pigskin of routine paraffin wax embedded section institutional framework photo, compare with Fig. 4, some adhesion of the fiber among Fig. 6, profile is difficult to be differentiated, and has the torsional deformation phenomenon to take place.
Above instance only is used to explain the present invention's usefulness; But not limitation of the present invention; The technician in relevant technologies field under the situation that does not break away from the spirit and scope of the present invention, can also make various conversion or modification; Therefore all technical schemes that are equal to also should belong to category of the present invention, should be limited each claim.
Claims (7)
1. leather sample preparation methods that is applicable to the metallography microscope sem observation, step is following:
(1) elder generation adds the promoter of 0.5～2 mass parts in the unsaturated polyester resin of 100 mass parts, stirs 5～10 minutes, and then adds the hardening agent of 1～3 mass parts; Stirred 5～10 minutes, and then, left standstill 8～15 minutes; The air that discharge is sneaked into obtains fixing resin;
(2) sample is immersed in the fixing resin that step (1) makes, after fixing resin infiltrates sample fully, takes out sample, in 60 ℃ of thermostatic drying chambers, solidified 1～2 hour, solidified sample;
(3) the solidified sample two ends that step (2) made polish, and are fixed in the mould fixing resin that implantation step in mould (1) makes then; 25 ℃ solidified 1～2 hour, and the demoulding obtains the appearance piece that the middle part is fixed with solidified sample; Solidified after 60 ℃ 1～2 hour, and got the back and solidify an appearance piece;
(4) the back curing appearance piece that step (3) is made makes the leather sample that is applicable to the metallography microscope sem observation after sand papering, polishing.
2. preparation method as claimed in claim 1; It is characterized in that; Unsaturated polyester resin in the said step (1) is that fiberglass is with adjacent benzene/metaphenylene unsaturated polyester resin or vinyl esters unsaturated polyester resin; Promoter is cobalt iso-octoate or cobalt naphthenate, and hardening agent is methyl ethyl ketone peroxide or cyclohexanone peroxide.
3. preparation method as claimed in claim 1 is characterized in that, adopts following method to make fixing resin infiltrate sample fully in the said step (2):
With the fixing resin that sample one end in contact step (1) makes, keep sample to stand on the fixing resin top then, left standstill 0.5～2 hour, fixing resin gets into interfibrous space in the sample, and the complete filling space, gets final product.
4. preparation method as claimed in claim 1 is characterized in that, the sample in the said step (2) is the leather bar of long 15～25mm, wide 1.5～2.5mm.
5. preparation method as claimed in claim 1 is characterized in that, the mould in the said step (3) is the cylindrical mold of internal diameter 30～50mm, high 15-25mm.
6. preparation method as claimed in claim 1 is characterized in that, the sand papering in the said step (4) is for use 200 orders, 320 orders, 500 orders, 1000 orders, 1500 orders, 2000 orders, 3000 order liquid honings successively.
7. preparation method as claimed in claim 1 is characterized in that, 150～300 rev/mins of metallurgical polishing machines that are finished in the said step (4) polished 1～2 minute.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102809563A (en) * | 2012-08-14 | 2012-12-05 | 广州市质量监督检测研究院 | Simple identification method for leather fiber structure |
| CN102928279A (en) * | 2012-11-13 | 2013-02-13 | 无锡江南计算技术研究所 | Metallographical sample-filling secondary glue filling method |
| CN103389240A (en) * | 2013-08-14 | 2013-11-13 | 齐鲁工业大学 | Device for obtaining leather section at compression state and sample preparation method |
| CN103398888A (en) * | 2013-08-14 | 2013-11-20 | 齐鲁工业大学 | Device for acquiring stretched-state leather sections and sample preparation method |
| CN103615986A (en) * | 2013-12-11 | 2014-03-05 | 山东轻工业学院 | Method for measuring interlayer spacing of leather sample cross section sequence image by using layer peeling method |
| CN103630438A (en) * | 2013-12-11 | 2014-03-12 | 山东轻工业学院 | Novel application of water to polishing stage of metallographical sample preparation method of leather sample and use method of water |
| CN103645084A (en) * | 2013-12-11 | 2014-03-19 | 山东轻工业学院 | Polishing solution for obtaining leather sectional views by using metallographic sample preparation method |
| CN103674953A (en) * | 2013-12-11 | 2014-03-26 | 山东轻工业学院 | Method for acquiring sequence diagrams of cross sections of leather sample |
| CN108254375A (en) * | 2017-12-29 | 2018-07-06 | 广州检验检测认证集团有限公司 | A kind of method for differentiating ox leather and buffalo leather |
| CN108709801A (en) * | 2018-04-16 | 2018-10-26 | 四川理工学院 | Under a kind of detection load in high polymer composite material filler dispersity method |
| CN111307804A (en) * | 2020-03-20 | 2020-06-19 | 山西钢科碳材料有限公司 | Method for measuring skin-core structure of polyacrylonitrile pre-oxidized fiber and carbon fiber by metallographic microscope |
| WO2022252441A1 (en) * | 2021-05-31 | 2022-12-08 | 齐鲁工业大学 | Mct section image-based three-dimensional reconstruction method for leather fiber bundle |
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Cited By (20)
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| CN102809563B (en) * | 2012-08-14 | 2016-05-25 | 广州市质量监督检测研究院 | A kind of facility distinguish method of leather fiber structure |
| CN102809563A (en) * | 2012-08-14 | 2012-12-05 | 广州市质量监督检测研究院 | Simple identification method for leather fiber structure |
| CN102928279B (en) * | 2012-11-13 | 2015-07-08 | 无锡江南计算技术研究所 | Metallographical sample-filling secondary glue filling method |
| CN102928279A (en) * | 2012-11-13 | 2013-02-13 | 无锡江南计算技术研究所 | Metallographical sample-filling secondary glue filling method |
| CN103389240A (en) * | 2013-08-14 | 2013-11-13 | 齐鲁工业大学 | Device for obtaining leather section at compression state and sample preparation method |
| CN103398888A (en) * | 2013-08-14 | 2013-11-20 | 齐鲁工业大学 | Device for acquiring stretched-state leather sections and sample preparation method |
| CN103389240B (en) * | 2013-08-14 | 2015-09-09 | 齐鲁工业大学 | A kind of device and method for making sample obtaining compressive state leather cross section |
| CN103630438A (en) * | 2013-12-11 | 2014-03-12 | 山东轻工业学院 | Novel application of water to polishing stage of metallographical sample preparation method of leather sample and use method of water |
| CN103674953A (en) * | 2013-12-11 | 2014-03-26 | 山东轻工业学院 | Method for acquiring sequence diagrams of cross sections of leather sample |
| CN103630438B (en) * | 2013-12-11 | 2015-07-29 | 齐鲁工业大学 | Water is in the novelty teabag in leather sample metallographic sample preparation method polishing stage and using method |
| CN103645084A (en) * | 2013-12-11 | 2014-03-19 | 山东轻工业学院 | Polishing solution for obtaining leather sectional views by using metallographic sample preparation method |
| CN103674953B (en) * | 2013-12-11 | 2016-03-16 | 山东轻工业学院 | A kind of method obtaining leather sample cross section sequence of pictures |
| CN103645084B (en) * | 2013-12-11 | 2016-05-18 | 齐鲁工业大学 | A kind of metallographic sample preparation method is obtained leather cross section picture polishing fluid |
| CN103615986A (en) * | 2013-12-11 | 2014-03-05 | 山东轻工业学院 | Method for measuring interlayer spacing of leather sample cross section sequence image by using layer peeling method |
| CN103615986B (en) * | 2013-12-11 | 2016-08-24 | 齐鲁工业大学 | Layer goes method to obtain the measuring method of leather sample cross section sequence of pictures interlamellar spacing |
| CN108254375A (en) * | 2017-12-29 | 2018-07-06 | 广州检验检测认证集团有限公司 | A kind of method for differentiating ox leather and buffalo leather |
| CN108709801A (en) * | 2018-04-16 | 2018-10-26 | 四川理工学院 | Under a kind of detection load in high polymer composite material filler dispersity method |
| CN108709801B (en) * | 2018-04-16 | 2020-09-22 | 四川理工学院 | Method for detecting dispersion state of filler in high polymer composite material under load |
| CN111307804A (en) * | 2020-03-20 | 2020-06-19 | 山西钢科碳材料有限公司 | Method for measuring skin-core structure of polyacrylonitrile pre-oxidized fiber and carbon fiber by metallographic microscope |
| WO2022252441A1 (en) * | 2021-05-31 | 2022-12-08 | 齐鲁工业大学 | Mct section image-based three-dimensional reconstruction method for leather fiber bundle |
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