CN101718647A - Preparation method of conductive scanning metallographic sample - Google Patents
Preparation method of conductive scanning metallographic sample Download PDFInfo
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- CN101718647A CN101718647A CN200910311372A CN200910311372A CN101718647A CN 101718647 A CN101718647 A CN 101718647A CN 200910311372 A CN200910311372 A CN 200910311372A CN 200910311372 A CN200910311372 A CN 200910311372A CN 101718647 A CN101718647 A CN 101718647A
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Abstract
The invention relates to a preparation method of a scanning metallographic sample, particularly to a preparation method of a conductive scanning metallographic sample. The invention solves the problems of no conductibility of the scanning metallographic sample, homogeneous distribution of a conductive filling material and poor adhesive property between the conductive filling material and a base material. The method comprises the following steps of: selecting ebonite dust as the base material; selecting carbon soot as the conductive filling material, and adding the ebonite dust and the carbon soot in the volume proportion of 5:(2-3) into a container containing alcohol; heating the container to the temperature of 100DEG C, and stirring for 30 minutes; pouring out the mixture out offrom the container, and drying at the temperature of 50-100DEG C; pulverizing a dried composite material; putting the prepared powder into a mould, heating to the temperature of 130-150DEG C, simultaneously applying pressure to the mould, and retaining heat and pressure for 8-10 minutes; and taking out a sample to finish the preparation of the metallographic sample. The invention improves the adhesive property between the conductive filling material and the base material, and the conductive filling material is homogeneously distributed; the metallographic sample has stable physical-mechanical performance.
Description
Technical field
The present invention relates to a kind of preparation method of scanning metallographic sample, belong to metallographic sample preparing technical field.
Background technology
Requiring the metallographic sample must conduct electricity with sample platform when doing scanning of materials Electronic Speculum metallographic observation is connected, and some scanning electron microscope metallographic observation samples are because a variety of causes need be processed into certain shape and size, classic method is tested metallographic sample to be put into the mould of definite shape, add organic polymer fillers such as bakelite powder or urea-formaldehyde moulding powder again, then plus-pressure and temperature is elevated to 120-130 ℃ of curing prepares sample.The sample of the method preparation has certain intensity and hardness, and preparation sample efficient height, price be low, be convenient to rubbing down processing.But, because filler is non-conductive, therefore when doing scanning of materials Electronic Speculum metallographic observation, must observed conduction sample be connected with sample platform by conductive rubber mud, make that scanning of materials Electronic Speculum metallographic observation efficient is low, and observing effect is bad.
Conducting polymer composite can be divided into structural conductive macromolecular material and conductive polymeric composite two big classes according to structure and preparation method's difference.Structural conductive macromolecular material (or claiming intrinsic macromolecule conducting material) is meant that molecular structure itself can conduct electricity or passes through the conjugated polymer that doping treatment has conducting function afterwards, as polyacetylene, polyaniline, polypyrrole, polythiophene, poly-furans etc., conductive polymeric composite is meant with the polymkeric substance to be matrix, by adding various electroconductive stuffings, and adopt compound not only the having certain conducting function but also having the heterogeneous composite material of excellent mechanical performances of making of physico-chemical process.The structural conductive macromolecular material obtain the less of practical application, and majority is a semiconductor material because the singularity of structure and the difficulty of preparation and purification also are in the laboratory study stage mostly at present.Conductive polymeric composite, basic identical, easy to prepare because of machine-shaping with general macromolecular material, stronger practicality is arranged, so comparatively widespread use.
The preparation method of conductive polymeric composite mainly contains three kinds: 1, surface treatment.Surface treatment is meant on the plastic polymer surface carries out conductive processing to reach higher conductance, comprises the metal thermal spraying method, coating process and conductive coating method.2, conductive filler lamination composite algorithm.The conductive filler laminated layer is legal be with wire netting, plate, silk, blanket etc. as middle layer, both sides plastic basis material or utilize double-deck parallel extrusion method to make one deck to be electroconductive resin on the lamination again, another layer is the double-layer product of ordinary resin.3, conductive filler disperses composite algorithm.Conductive filler disperses composite algorithm to be mainly used to make conductive rubber, conductive plastics, electrically-conducting paint, electro-conductive adhesive etc.It is to prepare the most frequently used method of conducing composite material that conductive filler disperses composite algorithm.The step of disperseing composite algorithm to prepare conducing composite material with conductive filler is: 1. select conductive filler and matrix material; 2. prepare burden; 3. blend; 4. moulding (extrude, injection moulding, mold pressing etc.); 5. electric performance test.The problem that conductive filler disperses composite algorithm to exist mainly contains: 1. the distribution of conductive filler in goods is often inhomogeneous, thereby makes manufactured goods conductivity everywhere inconsistent; 2. the cohesiveness between conductive filler and the matrix material is generally relatively poor, especially this situation is particularly evident when conductive filler content is higher, and the bonding between conductive filler and the matrix material is bad, and the mechanical property of the conducing composite material product after the moulding is descended greatly.Coupling agent and other processing aid of determining conductive filler and matrix material suitable proportioning and definite function admirable are the keys of preparation conducing composite material.
The used conductive additive of conductive polymeric composite mainly contains two classes: a class is an antistatic agent, and another kind of is various conducting fillers.Add antistatic agent and can only give material lower electric conductivity, antistatic agent can constantly be consumed, and makes that the serviceable life of material is short, and electric conductivity is subjected to the influence of environment such as temperature, humidity, friction etc. big.Thereby conductive polymeric composite is many to add various conducting fillers at present.Conductive filler plays an important role to the development of composite conductive plastic, and the selection of conductive filler is most important to design, the manufacturing of composite conductive plastic.Conductive filler commonly used has: 1. carbon charcoal series, and as graphite, carbon black and carbon fiber etc.2. metal series: as the powder of metal powder, fragment and fiber plating and fiber etc.3. other series is as inorganic salts and metal oxide powder etc.But existing conductive filler in use exposes many problems: the metal powder of general high dispersive does not have in plastics and is formed with the chain type organizational capacity that is beneficial to conduction; so usually the mass percent of metal will reach the resistivity that 40%-50% just can make material and begins to reduce; but high like this metal powder content not only costs an arm and a leg; be unsuitable for extensive use, usually the mechanical property of superpolymer significantly degenerated.The copper powder cheapness, but easily oxidized and form oxide film from the teeth outwards, the conductivity of conductive plastics is significantly reduced.In addition, high-density metal powder and corresponding more low-density high polymer material are difficult for forming equally distributed batch mixing, thereby these metal powders do not have very big use value; Carbon is filler good conductivity, good corrosion resistance, but easily deposition is lumpd, the difficult dispersion, and poor adhesive force, and color is dark, limits its use to a great extent.Because carbon black structure is stable, the surface is difficult for oxidation, and forms chain type or the reticular tissue that stretches easily in material.The outstanding feature of good conductive carbon black is that the particle diameter of primary granule is little, and it is high that porosity is wanted, and the ability that forms aggregation wants high.Except that above-mentioned character, the chemical composition of carbon blacksurface layer also can influence the electric conductivity of conductive material.The increasing of oxy radical on the surface can make the contact resistance between carbon black pellet increase, thereby the conductivity of conductive plastics is reduced.Graphite has lamellar structure, can realize that lamella is compound, reduces conductivity percolation threshold, descends but easily produce the concentrated strength of materials that makes of stress.How reducing the conductivity threshold of filled-type conductive polymer composite, is the key point of such investigation of materials.After the electric conductivity inserts reaches finite concentration, the physical-mechanical properties of material is significantly degenerated.Therefore, must the electric conductivity that the physical-mechanical properties of material and this goods are required combine consideration, the proportioning of each component of choose reasonable during actual the use.The compound-type conducting Development of Materials mainly concentrates on two aspects of combination property that improve conductivity and improve material.
Summary of the invention
The objective of the invention is that non-conductive, the conductive filler that conductive scanning metallographic sample exists is evenly distributed in order to solve, the problem of the bad adhesion between conductive filler and the matrix material, and then provide a kind of preparation method of conductive scanning metallographic sample.
The preparation method's of a kind of conductive scanning metallographic sample of the present invention step is:
Step 1: the choosing of raw material: choosing bakelite powder is matrix material; Carbon black is a conductive filler, and the bakelite powder of choosing and the volume ratio of carbon black are 5: (2-3);
Step 2: the preparation of powder: at first, be 5 with volume ratio: bakelite powder (2-3) and carbon black join in the container, and the alcohol identical with the bakelite powder volume is housed in the container; Then, container is put into water-bath be heated to 100 ℃, mechanical raking crude alcohol mixture 30 minutes; Again the potpourri that mixes is poured out container, oven dry obtains compound substance under 50-100 ℃ temperature range; At last, dried composite material is pulverized to the particle of particle diameter less than 3mm, finished the preparation of powder;
Step 3: the moulding of metallographic sample: at first, prepared powder is put into mould, mold heated to 130-150 ℃, is exerted pressure to mould according to the addition of powder simultaneously, then, heat-insulation pressure keeping 8-10 minute; At last, take out sample, finish the preparation of metallographic sample.
The present invention compared with prior art has following beneficial effect: the present invention adopts conductive filler to disperse composite algorithm, and the powder preparation is simple, and cost is low; The present invention and with alcohol as coupling agent, under suitable temperature, stir, not only solved conductive filler skewness problem, and shortened mixing time greatly, and improved cohesiveness between conductive filler and the matrix material; The present invention is that the organic polymer sample of conductive filler preparation can avoid the secondary on specimen preparation process surface to scratch the conductivity height with the carbon black; Adopt heating and metallographic sample moulding that the mode of carrying out simultaneously of exerting pressure prepares is easy, simple to operate, efficient is high, and physical-mechanical properties is stable, the metallographic sample is through electric performance test, resistivity＜130 Ω/cm
3
Embodiment
Embodiment one: the preparation method's of the conductive scanning metallographic sample of present embodiment step is:
Step 1: the choosing of raw material: choosing bakelite powder is matrix material; Carbon black is a conductive filler, and the bakelite powder of choosing and the volume ratio of carbon black are 5: (2-3);
Step 2: the preparation of powder: at first, be 5 with volume ratio: bakelite powder (2-3) and carbon black join in the container, and the alcohol identical with the bakelite powder volume is housed in the container; Then, container is put into water-bath be heated to 100 ℃, mechanical raking crude alcohol mixture 30 minutes; Again the potpourri that mixes is poured out container, oven dry obtains compound substance under 50-100 ℃ temperature range; At last, dried composite material is pulverized to the particle of particle diameter less than 3mm, finished the preparation of powder;
Step 3: the moulding of metallographic sample: at first, prepared powder is put into mould, mold heated to 130-150 ℃, is exerted pressure to mould according to the addition of powder simultaneously, then, heat-insulation pressure keeping 8-10 minute; At last, take out sample, finish the preparation of metallographic sample.
Embodiment two: what present embodiment and embodiment one were different is: the bakelite powder of choosing in the step 1 and the volume ratio of carbon black are 5: 2.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the bakelite powder of choosing in the step 1 and the volume ratio of carbon black are 5: 3.Other step and parameter are identical with embodiment one.
Embodiment four: what present embodiment and embodiment one to three were different is: in the step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 60 ℃ temperature range.Other step and parameter are identical with embodiment one to three.
Embodiment five: what present embodiment and embodiment one to three were different is: in the step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 70 ℃ temperature range.Other step and parameter are identical with embodiment one to three.
Embodiment six: what present embodiment and embodiment one to three were different is: in the step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 80 ℃ temperature range.Other step and parameter are identical with embodiment one to three.
Embodiment seven: what present embodiment and embodiment one to three were different is: in the step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 90 ℃ temperature range.Other step and parameter are identical with embodiment one to three.
Embodiment eight: what present embodiment and embodiment one to seven were different is: in the step 2 dried composite material pulverized for particle diameter be the particle of 2.5mm.Other step and parameter are identical with embodiment one to seven.
Embodiment nine: what present embodiment and embodiment one to seven were different is: in the step 2 dried composite material pulverized for particle diameter be the particle of 2mm.Other step and parameter are identical with embodiment one to seven.
Embodiment ten: what present embodiment and embodiment one to seven were different is: in the step 2 dried composite material pulverized for particle diameter be the particle of 1.5mm.Other step and parameter are identical with embodiment one to seven.
Embodiment 11: what present embodiment and embodiment one to seven were different is: in the step 2 dried composite material pulverized for particle diameter be the particle of 1mm.Other step and parameter are identical with embodiment one to seven.
Embodiment 12: what present embodiment and embodiment one to 11 were different is: mold heated to 140 ℃ in the step 3.Other step and parameter are identical with embodiment one to 11.
Embodiment 13: what present embodiment and embodiment one to 12 were different is: the time of heat-insulation pressure keeping is 9 minutes in the step 3.Other step and parameter are identical with embodiment one to 13.
Embodiment 14: what present embodiment and embodiment one to 13 were different is: the granularity＜3mm of the bakelite powder in the step 1.Be convenient to processing.Other step and parameter are identical with embodiment one to 14.
Claims (10)
1. the preparation method of a conductive scanning metallographic sample, it is characterized in that: preparation method's step is:
Step 1: the choosing of raw material: choosing bakelite powder is matrix material; Carbon black is a conductive filler, and the bakelite powder of choosing and the volume ratio of carbon black are 5: (2-3);
Step 2: the preparation of powder: at first, be 5 with volume ratio: bakelite powder (2-3) and carbon black join in the container, and the alcohol identical with the bakelite powder volume is housed in the container; Then, container is put into water-bath be heated to 100 ℃, mechanical raking crude alcohol mixture 30 minutes; Again the potpourri that mixes is poured out container, oven dry obtains compound substance under 50-100 ℃ temperature range; At last, dried composite material is pulverized to the particle of particle diameter less than 3mm, finished the preparation of powder;
Step 3: the moulding of metallographic sample: at first, prepared powder is put into mould, mold heated to 130-150 ℃, is exerted pressure to mould according to the addition of powder simultaneously, then, heat-insulation pressure keeping 8-10 minute; At last, take out sample, finish the preparation of metallographic sample.
2. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: the bakelite powder of choosing in the described step 1 and the volume ratio of carbon black are 5: 2.
3. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: the bakelite powder of choosing in the described step 1 and the volume ratio of carbon black are 5: 3.
4. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: in the described step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 60 ℃ temperature range.
5. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: in the described step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 70 ℃ temperature range.
6. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: in the described step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 80 ℃ temperature range.
7. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: in the described step 2 potpourri that mixes is poured out container, oven dry obtains compound substance under 90 ℃ temperature range.
8. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: in the described step 2 dried composite material pulverized for particle diameter be the particle of 2.5mm.
9. according to the preparation method of the described conductive scanning metallographic sample of claim 1, it is characterized in that: in the described step 2 dried composite material pulverized for particle diameter be the particle of 2mm.
10. according to the preparation method of claim 1,2,6 or 8 described conductive scanning metallographic samples, it is characterized in that: the granularity＜3mm of the bakelite powder in the described step 1.
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| CN200910311372A CN101718647A (en) | 2009-12-14 | 2009-12-14 | Preparation method of conductive scanning metallographic sample |
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| CN200910311372A CN101718647A (en) | 2009-12-14 | 2009-12-14 | Preparation method of conductive scanning metallographic sample |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101900647A (en) * | 2010-07-30 | 2010-12-01 | 西北有色金属研究院 | Micron-sized metal powder metallic phase mounting method |
| CN102507583A (en) * | 2011-11-02 | 2012-06-20 | 苏州华碧微科检测技术有限公司 | Microscopic observation method for microsection |
| CN103196730A (en) * | 2013-04-12 | 2013-07-10 | 哈尔滨工业大学 | Conducting anti-chamfering scanning electron microscope metallographic phase sample and preparation method thereof |
| CN103439156A (en) * | 2013-07-30 | 2013-12-11 | 国家电网公司 | Preparation method of laminating film for on-site metallographic examination of tower material |
| CN104568623A (en) * | 2014-08-13 | 2015-04-29 | 南京汉旗新材料科技有限公司 | Method for measuring hardness of biomass material |
-
2009
- 2009-12-14 CN CN200910311372A patent/CN101718647A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101900647A (en) * | 2010-07-30 | 2010-12-01 | 西北有色金属研究院 | Micron-sized metal powder metallic phase mounting method |
| CN102507583A (en) * | 2011-11-02 | 2012-06-20 | 苏州华碧微科检测技术有限公司 | Microscopic observation method for microsection |
| CN103196730A (en) * | 2013-04-12 | 2013-07-10 | 哈尔滨工业大学 | Conducting anti-chamfering scanning electron microscope metallographic phase sample and preparation method thereof |
| CN103196730B (en) * | 2013-04-12 | 2015-06-17 | 哈尔滨工业大学 | Conducting anti-chamfering scanning electron microscope metallographic phase sample and preparation method thereof |
| CN103439156A (en) * | 2013-07-30 | 2013-12-11 | 国家电网公司 | Preparation method of laminating film for on-site metallographic examination of tower material |
| CN104568623A (en) * | 2014-08-13 | 2015-04-29 | 南京汉旗新材料科技有限公司 | Method for measuring hardness of biomass material |
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Open date: 20100602 |