CN103808549A - Sample preparation method of scanning electron microscope of basalt fiber and asphalt mixed material fracture - Google Patents
Sample preparation method of scanning electron microscope of basalt fiber and asphalt mixed material fracture Download PDFInfo
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- CN103808549A CN103808549A CN201410086375.4A CN201410086375A CN103808549A CN 103808549 A CN103808549 A CN 103808549A CN 201410086375 A CN201410086375 A CN 201410086375A CN 103808549 A CN103808549 A CN 103808549A
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Abstract
The invention relates to a sample preparation method of a scanning electron microscope of a basalt fiber and asphalt mixed material fracture, which relates to the technical field of sample preparation of a material for testing of a scanning electron microscope. The method comprises the steps of first preparing an asphalt mixed material Marshall cylindrical test piece doped with basalt fibers by a Marshall standard compaction method, then cutting the cylindrical test piece to obtain bar-shaped test pieces, and cutting each of two opposite edges of each bar-shaped test piece of the mixed material along the height direction to form a small incision; performing water bath on the test pieces to achieve heat balance; and clamping two sides of the incisions of each test piece, fracturing the bar-shaped test piece of the mixed material and air-drying the fractured test piece. The obtained test piece fracture is relatively smooth, thus being favorable for the micro-observation on basalt fibers of the scanning electron microscope, so that the bonding situation between the basalt fibers and the asphalt mixed material and the reinforcement effect of the fibers during fracturing of the asphalt mixed material can be accurately mastered.
Description
technical field
The sample making technology that the present invention relates to scanning electron microscope test material, refers to the method for making sample that basalt fibre asphalt fracture is carried out to sem test especially.
Background technology
Basalt fibre is that natural basalt to be formed by volcanic eruption is as raw material, to after its fragmentation, join in melting furnaces, at 1450 ℃ ~ 1500 ℃ after melting, the continuous fiber forming by platinum-rhodium alloy bushing Defect, in whole production run, there is no the generation of industrial waste water, waste gas and other industrial refuses, be described as " new material of 21 century ".Basalt fibre was developed by Moscow glass and plastics research institute in 1954, within 1985, realized suitability for industrialized production in Ukraine, and within 2002, basalt fibre technology is put into China's 863 high-tech projects.In asphalt, basalt fibre, compared with other fibers, has that operating temperature range is large, mechanical property is excellent, chemical stability is good, ageing resistance is good, water stability is good and the outstanding advantage such as electric heating good insulation preformance.
Basalt fibre is different from polymer modified asphalt concrete to the impact of its mechanical property after joining in bituminous concrete matrix, and the length of basalt fibre and volume all can have obvious impact to mechanical behavior, Viscoelastic Mechanics performance before and after the usability of bituminous concrete matrix, cracking.Also adding of fiber can exert an influence to the micromechanism of asphalt, therefore the space existence of fiber in asphalt and and pitch between bonding situation all can have influence on macroscopical usability.
In the concrete Study on Microstructure of fibre reinforced asphalt, be mostly limited to the two-phase effect of fiber and pitch at present.Generally whether form new material by Infrared spectroscopy fiber and asphalt mastic interface, namely solve physical connection or chemistry connection, but the observation directly perceived of whether extracting in the time that destruction occurs bituminous concrete matrix for fiber or rupture is not seen, and current Infrared spectroscopy experimental study does not all relate to restraint condition and the fiber retardance situation in bituminous concrete matrix microfracture expansion of fiber to bituminous concrete inherent vice.
Scanning electron microscope is due to its high-resolution image measurement ability, extremely researcher's favor always in the microscopic appearance observation of material.Have researcher to use the bonding situation between the situation that is interspersed and fiber and the pitch of scanning electron microscope observation basalt fibre in asphalt, but method for making sample differ when current use scanning electron microscope observation, not unified standard.Traditional method for making sample is from asphalt cleavage fracture or fatigure failure rupture surface grab sample, and the size of each sample roughly approaches length × wide × height=3cm × 3cm × 2cm.The sample that the method is chosen is also under-represented, can not more comprehensively reflect the microstructure characteristic of whole rupture failure face and the basalt fibre distribution situation at the face of destruction, randomness while selection due to sample simultaneously, the size and shape of sample differs, and is unfavorable for observation and the comparative analysis of surface sweeping Electronic Speculum.
For the microstructure characteristic of further research basalt fibre asphalt section part and basalt fibre are in the distribution situation of section part, thereby seek the essence of the contribution of basalt fibre to asphalt mechanical property, need to use scanning electron microscope to carry out analytical test to sample destruction face.For obtaining the good analytical test result of true and accurate and reappearance, just need an opposed flattened and the unified fracture sample of shape size.
Summary of the invention
The object of the present invention is to provide the method for making sample of the scanning electron microscope of the basalt fibre asphalt fracture of the fracture sample that a kind of opposed flattened and shape size are unified.
Step of the present invention is as follows:
1) use the preparation of Marshall typical compacting method to mix the asphalt Marshall cylinder specimen of basalt fibre, specimen finish is 101.6mm ± 0.25mm, the high 63.5mm ± 1.3mm of being;
2) above-mentioned marshal piece is cut into the thin rounded flakes that thickness is 3～5mm;
3) each thin rounded flakes is cut, obtaining length is the compound bar-shaped sample that 30～35mm, the wide 10～15mm of being, height are 3～5mm;
4) respectively cut out a little otch in two opposite edges of compound bar-shaped sample along short transverse;
5) the compound bar-shaped sample with little otch is placed in to the water-bath 20～30 minutes of 5 ℃, makes specimen temperature and bath temperature reach thermal equilibrium;
6) take out compound bar-shaped sample, clamp respectively the both sides of sample otch, compound bar-shaped sample is broken disconnected;
7) be placed on room-dry by breaking disconnected sample.
Just obtain regular shape, the unified basalt fibre asphalt fracture sample of size by above method.
Principle of work of the present invention: asphalt is a kind of viscous-elastic material, along with the reduction of temperature, asphalt is changed to elasticity by stickiness gradually, under 5 ℃ of temperature conditions, compound Brittleness is remarkable, and the present invention utilizes this specific character of compound to carry out sample on the broken edge preparation.
Owing to having adopted such scheme, the present invention has the following advantages: 1) method for making sample is simple, easy to operate.With respect to traditional method for making sample, this method is without diametral compression test or the torture test of carrying out compound.2) regular shape, size unification.Destroy compared with the different fritter shape test specimen that section part peels off by choosing at random large test specimen with classic method, the fracture specimen shape size that this method is made is relatively uniform, strengthens the reappearance that Electronic Speculum is taken pictures.3) the fracture surface of sample opposed flattened obtaining, obtain the electromicroscopic photograph that basalt fibre clear and that reappearance is good distributes, be beneficial to the microcosmic observation to basalt fibre of scanning electron microscope, be convenient to correctly be familiar with between basalt fibre and asphalt by bonding situation and the reinforced action of fiber in the time that asphalt ftractures.
The applicable basalt fibre of the present invention can make the short basalt fibre of cutting, and can be also cotton-shaped basalt fibre.
In addition, air-dry time of the present invention is not less than 24h.Sample need to do processed in the time of electron microscopy observation, to guarantee to obtain observed image clearly.More than air-dry 24 hours can guarantee that in sample, moisture fully evaporates, and it is easy to operate to compare other dewatering types, saves energy consumption.Meanwhile, the accuracy while using the non-natural-dehydration modes such as baking oven heating may affect electron microscopy observation appearance of fracture.Therefore, the present invention selects air-dry more than 24 hours.
Described cutting adopts low speed diamond circular saw.Low speed diamond circular saw can cut the various solid materials material of easy damaged (especially superhard, frangible) under stabilized (steady-state) speed, and can cause hardly sample distortion, damaged and damage.Therefore, adopt low speed diamond circular saw can fully guarantee that in asphalt, basalt fibre can not occur heavily to distribute because of cutting sample, guarantee with this accuracy of observing.
Accompanying drawing explanation
Fig. 1 is basalt fibre asphalt thin rounded flakes sample structure schematic diagram.
Fig. 2 is basalt fibre asphalt bar-shaped sample structural representation.
Fig. 3,4 is respectively the sample Electronic Speculum pictures taken of utilizing the actual preparation of SEM sample preparation method that the present invention relates to a kind of basalt fibre asphalt fracture.
Fig. 5,6,7,8 is respectively the sample Electronic Speculum pictures taken of utilizing classic method to prepare.
In Fig. 1,2,3,1 is Irish touchstone asphalt matrix, and 2 is basalt fibre, and 3 for gathering materials, and 4 is asphalt mastic, and 5 is otch.
Embodiment
One, method for making sample of the present invention:
(1) use the preparation of Marshall typical compacting method to mix the asphalt marshal piece of basalt fibre, sample is cylindrical, and diameter is 101.6mm, the high 63.5mm of being.
(2) because marshal piece is larger, and scanning electron microscope example chamber size is less, so need to first obtain a undersized basalt fibre asphalt sample, use hi-precision cutting instrument that marshal piece is cut into the thin rounded flakes that thickness is 5mm, as shown in Figure 1.
(3) fine cut: use hi-precision cutting instrument equidistantly to cut asphalt thin rounded flakes along dotted line direction in Fig. 1, again bar-shaped sample two ends circular arc portion is cut, obtaining long is 30mm, the wide basalt fibre asphalt bar-shaped sample for 12mm, the high 5mm of being, as shown in Figure 2.
(4) use hi-precision cutting instrument respectively to cut out a little otch 5 at the relative position of two opposite edges of compound bar-shaped sample along short transverse.
(5) basalt fibre asphalt bar-shaped sample being put into maintenance in the water-bath of 5 ℃, about 30 minutes, makes specimen temperature and bath temperature reach thermal equilibrium.
(6) take out basalt fibre asphalt bar-shaped sample, with two pairs of clean pliers, clamp respectively the both sides of sample otch, firmly break disconnected.
(7) again sample is placed on to room-dry, air-dry 24h, obtains regular shape, the unified basalt fibre asphalt fracture sample of size.
The basalt fibre asphalt fracture sample that uses above-mentioned steps to obtain is carried out to surface sweeping electron microscopy observation, take as shown in Figure 3,4: the basalt fibre in compound is pulled off at incision position, the fiber stress that can well transmit and dissipate can be effectively described, overcome intergranular relative slippage.
Two, traditional sample preparation method:
1, the asphalt marshal piece of basalt fibre is mixed in the preparation of Marshall typical compacting method, and sample is cylindrical, and diameter is 101.6mm, the high 63.5mm of being.
2, cylinder specimen is put in the water-bath of 15 ℃ to maintenance 6 hours, made specimen temperature and bath temperature reach thermal equilibrium.
3, sample is placed in to Marshall Instrument for Pressure, pressurization, makes sample disjunction up and down.
4, scanning electron microscope observation is carried out in the cross section of fracture, Fig. 5,6,7,8 is shown in by the scanning electron microscope observation picture of taking, due to the randomness of classic method sampling and the scrambling of sample, take the picture otherness obtaining larger, can not prove fully enhancing and the toughening effect of basalt fibre at asphalt.
Claims (3)
1. the method for making sample of the scanning electron microscope of basalt fibre asphalt fracture, is characterized in that step is as follows:
1) use the preparation of Marshall typical compacting method to mix the asphalt Marshall cylinder specimen of basalt fibre, specimen finish is 101.6mm ± 0.25mm, the high 63.5mm ± 1.3mm of being;
2) above-mentioned marshal piece is cut into the thin rounded flakes that thickness is 3～5mm;
3) each thin rounded flakes is cut, obtaining length is the compound bar-shaped sample that 30～35mm, the wide 10～15mm of being, height are 3～5mm;
4) respectively cut out a little otch in two opposite edges of compound bar-shaped sample along short transverse;
5) the compound bar-shaped sample with little otch is placed in to the water-bath 20～30 minutes of 5 ℃, makes specimen temperature and bath temperature reach thermal equilibrium;
6) take out compound bar-shaped sample, clamp respectively the both sides of sample otch, compound bar-shaped sample is broken disconnected;
7) be placed on room-dry by breaking disconnected sample.
2. method for making sample according to claim 1, is characterized in that air-dry time is not less than 24h.
3. method for making sample according to claim 1, is characterized in that described cutting adopts low speed diamond circular saw.
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| CN201410086375.4A CN103808549A (en) | 2014-03-11 | 2014-03-11 | Sample preparation method of scanning electron microscope of basalt fiber and asphalt mixed material fracture |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067406A (en) * | 2015-08-14 | 2015-11-18 | 中国石油化工股份有限公司 | Argon ion polishing/scanning electron microscope analyzing and sampling method for shale samples |
| CN105842027A (en) * | 2016-03-23 | 2016-08-10 | 武汉理工大学 | Preparation method of asphalt mixture sample ultrathin slice for microscopic observation |
| CN106442032A (en) * | 2015-08-07 | 2017-02-22 | 中国科学院宁波材料技术与工程研究所 | Scanning electron microscopy sample production method of coated white cardboard fracture |
| CN108593691A (en) * | 2018-04-24 | 2018-09-28 | 扬州大学 | A kind of fracture method for making sample based on basalt fibre pitch mixed material cracking resistance |
| CN111060504A (en) * | 2019-12-09 | 2020-04-24 | 扬州大学 | Asphalt mixture basalt fiber observation method and test piece |
| CN112326705A (en) * | 2020-11-30 | 2021-02-05 | 天津海关化矿金属材料检测中心 | Qualitative identification method of basalt fibers |
| CN114014587A (en) * | 2021-11-16 | 2022-02-08 | 辽宁省交通规划设计院有限责任公司 | Preparation and analysis method of basalt fiber transparent mixture |
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| JP2004212271A (en) * | 2003-01-07 | 2004-07-29 | Hitachi High-Technologies Corp | Method and apparatus for preparing fracture sample and sample observation method |
| CN102798556A (en) * | 2012-07-05 | 2012-11-28 | 首钢总公司 | Alloyed galvanized sheet zinc layer brittle fracture preparation device and experimental method |
| CN103185676A (en) * | 2011-12-27 | 2013-07-03 | 国家纳米技术与工程研究院 | Sample preparation method for fracture of tungsten carbide coating on magnesium-alloy surface via scanning electron microscope |
| CN103344473A (en) * | 2013-07-15 | 2013-10-09 | 东南大学 | Method for molding asphalt mixture specimen for test by using rotary compaction method |
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2014
- 2014-03-11 CN CN201410086375.4A patent/CN103808549A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004212271A (en) * | 2003-01-07 | 2004-07-29 | Hitachi High-Technologies Corp | Method and apparatus for preparing fracture sample and sample observation method |
| CN103185676A (en) * | 2011-12-27 | 2013-07-03 | 国家纳米技术与工程研究院 | Sample preparation method for fracture of tungsten carbide coating on magnesium-alloy surface via scanning electron microscope |
| CN102798556A (en) * | 2012-07-05 | 2012-11-28 | 首钢总公司 | Alloyed galvanized sheet zinc layer brittle fracture preparation device and experimental method |
| CN103344473A (en) * | 2013-07-15 | 2013-10-09 | 东南大学 | Method for molding asphalt mixture specimen for test by using rotary compaction method |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442032A (en) * | 2015-08-07 | 2017-02-22 | 中国科学院宁波材料技术与工程研究所 | Scanning electron microscopy sample production method of coated white cardboard fracture |
| CN105067406A (en) * | 2015-08-14 | 2015-11-18 | 中国石油化工股份有限公司 | Argon ion polishing/scanning electron microscope analyzing and sampling method for shale samples |
| CN105842027A (en) * | 2016-03-23 | 2016-08-10 | 武汉理工大学 | Preparation method of asphalt mixture sample ultrathin slice for microscopic observation |
| CN108593691A (en) * | 2018-04-24 | 2018-09-28 | 扬州大学 | A kind of fracture method for making sample based on basalt fibre pitch mixed material cracking resistance |
| CN111060504A (en) * | 2019-12-09 | 2020-04-24 | 扬州大学 | Asphalt mixture basalt fiber observation method and test piece |
| CN111060504B (en) * | 2019-12-09 | 2022-04-08 | 扬州大学 | Asphalt mixture basalt fiber observation method and test piece |
| CN112326705A (en) * | 2020-11-30 | 2021-02-05 | 天津海关化矿金属材料检测中心 | Qualitative identification method of basalt fibers |
| CN112326705B (en) * | 2020-11-30 | 2023-01-13 | 天津海关化矿金属材料检测中心 | Qualitative identification method of basalt fibers |
| CN114014587A (en) * | 2021-11-16 | 2022-02-08 | 辽宁省交通规划设计院有限责任公司 | Preparation and analysis method of basalt fiber transparent mixture |
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Application publication date: 20140521 |