CN103822933A - Fiber number measurement method for carbon fiber multifilament - Google Patents
Fiber number measurement method for carbon fiber multifilament Download PDFInfo
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- CN103822933A CN103822933A CN201210464385.8A CN201210464385A CN103822933A CN 103822933 A CN103822933 A CN 103822933A CN 201210464385 A CN201210464385 A CN 201210464385A CN 103822933 A CN103822933 A CN 103822933A
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Abstract
The invention belongs to a physical-chemical testing technology, and relates to a fiber number measurement method for a carbon fiber multifilament. A scanning electron microscope is used for analysis, and the fiber number measurement method for the carbon fiber multifilament comprises sampling, sample preparation, cold embedding of a test sample, polishing of the test sample, placement of the test sample, vacuumizing of the scanning electron microscope, parameter regulation of the scanning electron microscope, low-vacuum photographing of the scanning electron microscope, measurement of the number of fibers and calculation of a test result. According to the method, the fiber number of the carbon fiber multifilament can be accurately detected and analyzed, and the requirements for scientific research production and failure analysis are met.
Description
Technical field
The invention belongs to physical and chemical testing technology, relate to a kind of carbon fiber multifilament fiber radical assay method.
Background technology
Carbon fiber multifilament fiber radical is measured and is carried out GB3363-82 Test method for number of filaments in carbon fiber strands by microscopy (microscopic method) always, this standard-required is photographed under optical microscope, on photo, press counter with color pencil by electronic calculator or hand, the fiber comprising in multifilament is counted by root.In actual testing process, this state's calibration method operability is very poor, on the photo that utilizes optical microscope to take, counts and looks into number of fiber, while looking into number of fiber, many owing to counting, multiple is low, close and numerous, manually look into number and very easily make mistakes, be not suitable for detecting in production run.
Summary of the invention
The technical problem to be solved in the present invention:
The present invention proposes a kind of carbon fiber multifilament fiber radical assay method, to meet the needs of research and production and failure analysis.
Technical scheme of the present invention:
Carbon fiber multifilament fiber radical assay method, this method comprises the following steps:
1.1 samplings, can select following two kinds of forms sampling:
1.1.1 the first: from tested carbon fiber multifilament sample, cut at random one section of multifilament of long 450mm-520mm as sample, except product technology condition separately has regulation, every batch of carbon fiber got a sample from three;
1.1.2 the second: get the carbon fiber multifilament tensile sample of two gluings as test samples;
1.2 sample preparations:
1.2.1 the preparation of the first sampled form multifilament sample, one section, the long 450mm-520mm multifilament of clip; Clamp two sections, multifilament with clip, in binder solution, flood 1-2 minute, take out and be hung on framework, at room temperature hang 2 to 4h, then in the thermostatic drying chamber of 80 ℃, be incubated 2 to 4h;
1.2.2 the second form multifilament sample directly uses;
The cold of 1.3 samples inlayed:
1.3.1 the multifilament of gluing is cut into some segments of long 20-25mm, and is bundled into a branch ofly with tinsel, utilize cold pointing machine, be coldly embedded in suitable cold inlaying in agent;
Polishing of 1.4 samples:
1.4.1 the cold sample of having inlayed is used successively to waterproof abrasive paper from coarse to fine wet-milling under circulating water on metallographic pre-mill; Then on buffing machine, use polishing fabric and antiscuffing paste polishing, the dirt that test piece examine surface is observed without impact;
1.4.2 by polished sample, on metallic phase polisher milling, with clean polishing fabric and the careful washed samples of circulating water surface;
1.5 lay sample: by the sample preparing, put on the indoor sample stage of scanning electron microscope example;
1.6 scanning electron microscope vacuumize; Select low vacuum pattern, equipment automatic vacuum, pressure is 60.00MPa;
1.7 adjust scanning electron microscope parameter; Moving stage, make sample topmost apart from electron gun lower surface 10mm-12mm, mode adjustment is arrived to secondary electron pattern, the 20.00KV that adds high pressure, selecting light beam is φ 4.0, enlargement factor is 1000 times to 1500 times, adjusting focal length, brightness 44.0, contrast 70.0, scanning electron microscope image is in clear state;
1.8 scanning electron microscope low vacuum photographies are absorbed photo under selected multiple, and photo comprises 25 multifilament fibers, is used for measuring the fibre single thread radical that every fiber multifilament comprises;
The mensuration of 1.9 number of fiber, to fibre single thread radical every piece multifilament observation area in counts on the photo absorbing under corresponding multiple, records respectively the radical of monofilament in 25 multifilament; The fiber comprising in multifilament is counted by root; The double result of counting, differs and should be less than 0.5%;
1.10 calculate test findings: take the mean value of the each sample multifilament fiber radical of surveyed and maximal value, minimum value as test result.
In 1.3 described steps, available adhesive cool is inlayed.
Beneficial effect of the present invention:
The present invention can carry out accurately detecting and analyzing to carbon fiber multifilament fiber radical, has met the needs of research and production and failure analysis.
Embodiment
Below the present invention is described in further details.
Carbon fiber multifilament fiber radical assay method, this method adopts scanning electron microscope to analyze, and it is as follows that carbon fiber multifilament fiber radical is measured concrete analysis step:
1.1 samplings: can select two kinds of form samplings;
1.1.1 the first: in one bag of carbon determination fiber multifilament sample, cut at random the one section of multifilament that is about 500mm as sample, except product technology condition separately has regulation, every batch of carbon fiber got a sample from three.
1.1.2 the second: get the carbon fiber multifilament tensile sample of two gluings as test samples.
1.2 sample preparation
1.2.1 the preparation of the first sampled form multifilament sample, clip is about one section, 500mm multifilament; Clamp two sections, multifilament with clip, in binder solution, flood approximately 1 minute, take out and be hung on framework, at room temperature hang 2 to 4h, then in the thermostatic drying chamber of 80 ℃, be incubated 2 to 4h.
1.2.2 the second form multifilament sample directly uses.
The cold of 1.3 samples inlayed;
1.3.1 the multifilament of gluing is cut into the some segments that are about 20mm, and is bundled into a branch ofly with tinsel, utilize cold pointing machine, be coldly embedded in suitable cold inlaying in agent; Available adhesive cool is inlayed, and also can inlay with other materials is cold.
Polishing of 1.4 samples
1.4.1 the cold sample of having inlayed is used successively to waterproof abrasive paper from coarse to fine wet-milling under circulating water on metallographic pre-mill.Thereafter on buffing machine, use polishing fabric and antiscuffing paste polishing, the dirt that test piece examine surface is observed without impact;
1.4.2 by polished sample, on metallic phase polisher milling, with clean polishing fabric and the careful washed samples of circulating water surface.
1.5 lay sample; By the sample preparing, put on the indoor sample stage of scanning electron microscope example;
1.6 scanning electron microscope vacuumize; Select low vacuum pattern, equipment automatic vacuum, pressure 60.00MPa;
1.7 adjust scanning electron microscope parameter; Moving stage, makes sample topmost apart from electron gun lower surface 10mm, and by mode adjustment, to secondary electron pattern, 20.00KV adds high pressure, selecting light beam is φ 4.0, and enlargement factor is 1000 times to 1500 times, adjusting focal length, brightness 44.0, contrast 70.0, scanning electron microscope image is in clear state;
1.8 scanning electron microscope low vacuum photographies are absorbed photo under selected multiple, and photo comprises 25 multifilament fibers, is used for measuring the fibre single thread radical that every fiber multifilament comprises.
The mensuration of 1.9 number of fiber, to fibre single thread radical every piece multifilament observation area in counts on the photo absorbing under corresponding multiple, records respectively the radical of monofilament in 25 multifilament.The fiber comprising in multifilament is counted by root.The double result of counting, differs and should be less than 0.5%.
1.10 calculate test findings: take the mean value of the each sample multifilament fiber radical of surveyed and maximal value, minimum value as test result.
Embodiment 1.Material standard DBC34-11, carries out determination and analysis to carbon fiber without latitude band multifilament fiber radical.
1. test procedure
1.1 sampling
The second sampled form: get the about 500mm of carbon fiber multifilament tensile sample of two gluings as test samples.
1.2 sample preparation
The multifilament of gluing is cut into 25 segments that are about 20mm.
The cold of 1.3 samples inlayed;
1.3.1 25 multifilament segment tinsels of having cut are bundled into a branch ofly, utilize that cold pointing machine is cold is embedded in suitable cold inlaying in agent.
1.4 polishing of sample
1.4.1 the cold sample of having inlayed is used successively to waterproof abrasive paper from coarse to fine wet-milling under circulating water on metallographic pre-mill.Thereafter on buffing machine, use polishing fabric and antiscuffing paste polishing, the dirt that test piece examine surface is observed without impact;
1.4.2 by polished sample, on metallic phase polisher milling, with clean polishing fabric and the careful washed samples of circulating water surface.
1.5 lay sample; By the sample preparing, put on the indoor sample stage of scanning electron microscope example;
1.6 scanning electron microscope vacuumize; Select low vacuum pattern, equipment automatic vacuum, pressure 60.00MPa;
1.7 adjust scanning electron microscope parameter; Moving stage, makes sample topmost apart from electron gun lower surface 10mm, and by mode adjustment, to secondary electron pattern, 20.00KV adds high pressure, selecting light beam is φ 4.0, and enlargement factor is 1200 times, adjusting focal length, brightness 44.0, contrast 70.0, scanning electron microscope image is in clear state;
1.8 scanning electron microscope low vacuum photographies are absorbed photo under 1200 times, and photo comprises 25 multifilament fibers, is used for measuring the fibre single thread radical that every fiber multifilament comprises.
1.9 the mensuration of number of fiber is counted to the fibre single thread radical in every multifilament in observation area on the photo of picked-up under 1200 times, the radical that records respectively monofilament in 25 multifilament is: 134,136,138,138,138,133.132,135,135,136,136,136,134,134,134,135,136,136,137,137,135,135,134,134,134.The double result of counting, differs in 0.5%.
1.10 calculating test findings
This sample multifilament fiber radical maximal value is 138,
This sample multifilament fiber radical minimum value is 132,
This sample multifilament fiber radical mean value is 135 (mean values 135.32).
Claims (2)
1. carbon fiber multifilament fiber radical assay method, is characterized in that, this method comprises the following steps:
1.1 samplings, can select following two kinds of forms sampling:
1.1.1 the first: from tested carbon fiber multifilament sample, cut at random one section of multifilament of long 450mm-520mm as sample, except product technology condition separately has regulation, every batch of carbon fiber got a sample from three;
1.1.2 the second: get the carbon fiber multifilament tensile sample of two gluings as test samples;
1.2 sample preparations:
1.2.1 the preparation of the first sampled form multifilament sample, one section, the long 450mm-520mm multifilament of clip; Clamp two sections, multifilament with clip, in binder solution, flood 1-2 minute, take out and be hung on framework, at room temperature hang 2 to 4h, then in the thermostatic drying chamber of 80 ℃, be incubated 2 to 4h;
1.2.2 the second form multifilament sample directly uses;
The cold of 1.3 samples inlayed:
1.3.1 the multifilament of gluing is cut into some segments of long 20-25mm, and is bundled into a branch ofly with tinsel, utilize cold pointing machine, be coldly embedded in suitable cold inlaying in agent;
Polishing of 1.4 samples:
1.4.1 the cold sample of having inlayed is used successively to waterproof abrasive paper from coarse to fine wet-milling under circulating water on metallographic pre-mill; Then on buffing machine, use polishing fabric and antiscuffing paste polishing, the dirt that test piece examine surface is observed without impact;
1.4.2 by polished sample, on metallic phase polisher milling, with clean polishing fabric and the careful washed samples of circulating water surface;
1.5 lay sample: by the sample preparing, put on the indoor sample stage of scanning electron microscope example;
1.6 scanning electron microscope vacuumize; Select low vacuum pattern, equipment automatic vacuum, pressure is 60.00MPa;
1.7 adjust scanning electron microscope parameter; Moving stage, make sample topmost apart from electron gun lower surface 10mm-12mm, mode adjustment is arrived to secondary electron pattern, the 20.00KV that adds high pressure, selecting light beam is φ 4.0, enlargement factor is 1000 times to 1500 times, adjusting focal length, brightness 44.0, contrast 70.0, scanning electron microscope image is in clear state;
1.8 scanning electron microscope low vacuum photographies are absorbed photo under selected multiple, and photo comprises 25 multifilament fibers, is used for measuring the fibre single thread radical that every fiber multifilament comprises;
The mensuration of 1.9 number of fiber, to fibre single thread radical every piece multifilament observation area in counts on the photo absorbing under corresponding multiple, records respectively the radical of monofilament in 25 multifilament; The fiber comprising in multifilament is counted by root; The double result of counting, differs and should be less than 0.5%;
1.10 calculate test findings: take the mean value of the each sample multifilament fiber radical of surveyed and maximal value, minimum value as test result.
2. carbon fiber multifilament fiber radical assay method as claimed in claim 1, is characterized in that, in 1.3 described steps, available adhesive cool is inlayed.
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| CN201210464385.8A CN103822933A (en) | 2012-11-16 | 2012-11-16 | Fiber number measurement method for carbon fiber multifilament |
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| CN201210464385.8A CN103822933A (en) | 2012-11-16 | 2012-11-16 | Fiber number measurement method for carbon fiber multifilament |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105043840A (en) * | 2015-09-21 | 2015-11-11 | 核工业理化工程研究院 | Large-tow carbon fiber tensile sample manufacturing method |
| CN105910856A (en) * | 2016-04-06 | 2016-08-31 | 哈尔滨飞机工业集团有限责任公司 | Preparation method for fine wire metallographic sample |
| CN114280280A (en) * | 2021-12-24 | 2022-04-05 | 中复神鹰碳纤维股份有限公司 | Method for testing number of carbon fiber multifilament |
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| JP2006294632A (en) * | 2006-06-08 | 2006-10-26 | Hitachi Ltd | Sample analysis method and device |
| CN101672810A (en) * | 2009-09-14 | 2010-03-17 | 哈尔滨飞机工业集团有限责任公司 | Method for analyzing composition uniformity of rubber material |
| CN101825587A (en) * | 2010-04-15 | 2010-09-08 | 哈尔滨飞机工业集团有限责任公司 | Fiber volume content test method of glass fiber laminated board |
| CN102445410A (en) * | 2011-09-19 | 2012-05-09 | 哈尔滨飞机工业集团有限责任公司 | Test method for pore content of carbon fiber reinforced plastic laminated plate |
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2012
- 2012-11-16 CN CN201210464385.8A patent/CN103822933A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006294632A (en) * | 2006-06-08 | 2006-10-26 | Hitachi Ltd | Sample analysis method and device |
| CN101672810A (en) * | 2009-09-14 | 2010-03-17 | 哈尔滨飞机工业集团有限责任公司 | Method for analyzing composition uniformity of rubber material |
| CN101825587A (en) * | 2010-04-15 | 2010-09-08 | 哈尔滨飞机工业集团有限责任公司 | Fiber volume content test method of glass fiber laminated board |
| CN102445410A (en) * | 2011-09-19 | 2012-05-09 | 哈尔滨飞机工业集团有限责任公司 | Test method for pore content of carbon fiber reinforced plastic laminated plate |
Non-Patent Citations (1)
| Title |
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| 国家标准局: "《中华人民共和国国家标准 GB3363-82》", 28 December 1982 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105043840A (en) * | 2015-09-21 | 2015-11-11 | 核工业理化工程研究院 | Large-tow carbon fiber tensile sample manufacturing method |
| CN105910856A (en) * | 2016-04-06 | 2016-08-31 | 哈尔滨飞机工业集团有限责任公司 | Preparation method for fine wire metallographic sample |
| CN105910856B (en) * | 2016-04-06 | 2018-08-24 | 哈尔滨飞机工业集团有限责任公司 | A kind of preparation method of fine wire metallographic specimen |
| CN114280280A (en) * | 2021-12-24 | 2022-04-05 | 中复神鹰碳纤维股份有限公司 | Method for testing number of carbon fiber multifilament |
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Application publication date: 20140528 |