CN109946130A - A kind of preparation method of micrometer level porous ceramic metallographic specimen - Google Patents
A kind of preparation method of micrometer level porous ceramic metallographic specimen Download PDFInfo
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- CN109946130A CN109946130A CN201910192537.5A CN201910192537A CN109946130A CN 109946130 A CN109946130 A CN 109946130A CN 201910192537 A CN201910192537 A CN 201910192537A CN 109946130 A CN109946130 A CN 109946130A
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Abstract
The invention discloses a kind of preparation methods of micrometer level porous ceramic metallographic specimen, the following steps are included: porous ceramics is put into mold by (a), then spackling is poured into mold, the spackling is mainly made of epoxy resin and curing agent according to the ratio that mass ratio is 1-3:1, then 4-8 hours are stood in a natural environment, Sample A is made;(b) Sample A is taken out, is polished directly, the micrometer level porous ceramic metallographic specimen is made.The average pore size of the porous ceramics is 2-20 μm.Compared with the existing technology, preparation process of the present invention is simple, and preparation cost is very low;In addition, metallographic specimen mechanical strength prepared by the present invention is good, wearability is good, surfacing, pass through metallographic microscope energy clear view metallographic specimen internal structure, applied to the quality testing in porous ceramics preparation process, it is advantageous to reduce the production cost that porous ceramics prepares qualified composite material or final products.
Description
Technical field
The invention belongs to ceramic metallographic field of sample preparation, in particular to a kind of system of micrometer level porous ceramic metallographic specimen
Preparation Method.
Background technique
In the research of Ceramic Reinforced MMCs, precast framework of the porous ceramics as composite material is burnt
Quality after knot directly affects the performance of final composite material.The uniformity of this kind of porous ceramics internal particle distribution is to material
It can influence greatly, if porous ceramics internal particle is unevenly distributed, directly just be used to prepare composite material, then make final products
Performance be unsatisfactory for actual requirement, need to prepare porous ceramics again, such economic cost and time cost are all very big.Therefore
To the observation of porous ceramics interior tissue pattern, very it is necessary to be conducive to prepare qualified composite material or final products.
Due to the limitation of optical microscopy focus adjustment, height is required to the processing quality on cellular ceramic sample surface,
Cellular ceramic sample surface flatness with higher is sought, and sample interior does not have between jljl phase under an optical microscope
Clearly interface.General cellular ceramic sample is difficult to meet these requirements.It is more to observe that metallographic microscope is generallyd use in industry
Institutional framework inside the ceramics sample of hole.Therefore need to prepare the metallographic specimen of porous ceramics.Metallographic specimen in the prior art
Preparation need by abrasive polishing process, but the bond strength between porous ceramic particles in the prior art is generally low, nothing
Method is polished directly processing.Conventional method is using the material after porous ceramics and metal composite as metallographic specimen, Neng Gouman
The requirement of sufficient metallographic specimen, but technique realizes complicated, higher cost, and the metallographic specimen quality prepared is also unstable.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of micrometer level porous ceramic metallographic specimen.System
Standby process is simple, and preparation cost is low, and the micrometer level porous ceramic metallographic sample performance of preparation is stablized, and wearability and bending strength are aobvious
Writing improves.
A kind of preparation method of micrometer level porous ceramic metallographic specimen, comprising the following steps:
(a) porous ceramics is put into mold, spackling is then poured into mold, the spackling is mainly by asphalt mixtures modified by epoxy resin
Rouge and curing agent are formed according to the ratio that mass ratio is 1-3:1 (preferably 2:1), then in a natural environment (or at room temperature) quiet
It sets 4-8 hours (preferably 6 hours), Sample A is made;
(b) Sample A is taken out, is polished directly, the micrometer level porous ceramic metallographic specimen is made.
Preferably, the porous ceramics is porous silicon carbide ceramic.
Preferably, the average pore size of the porous ceramics is 2-20 μm of (further preferred 8-20 μm, still more preferably 15
μm)。
Preferably, the size of porous ceramics described in step (a) is 10-30mm (length) × 10-30mm (width) × 1-
5mm (height), further preferred 20mm × 20mm × 2-3mm.The porous ceramics can be blocky (such as cubic block), such as will
The porous ceramics of certain size is cut into certain shape, such as is cut into blocky or other shapes.
Further, the mold includes mould sleeve 1, mold base 3, and the mould sleeve 1 is connect with mold base 3
Together, it such as is fixedly connected or is socketed.The sleeve 1 of the mold is circle, interior diameter 15-35mm, preferably 25mm, sleeve
Height 10-20mm, preferably 15mm, sleeve wall thickness 2-10mm, preferably 5mm.The fit tolerance of mold base 3 and sleeve is 0.1mm,
Mold base boss height is 2mm.
Preferably, the process poured into described in step (a) is to pour into spackling along the upper surface of porous ceramics, directly
Liquid level to spackling is higher than porous ceramics upper surface (or the highest point put) 4-10mm (preferably 5mm).Spackling is along more
The upper surface of hole ceramics, which pours into immerse under the effect of gravity in ceramic hole, forms complex.
Preferably, the epoxy resin is bisphenol A type epoxy resin, and the epoxide number of the epoxy resin is 0.41-
0.47mol/100g (is provided, model E44 (6101)) by Xingchen Synthetic Matrials Co., Ltd., Nantong.
Preferably, the curing agent is epoxy curing agent, it is further preferred that the epoxy curing agent is low
Molecular polyamide, such as 650 Versamids (650 represent the model of Versamid), 650 Versamid
Molecular weight be 600-1100.
Preferably, the material of the mold is aluminium alloy.
The spackling is liquid, the spackling leaving no air bubbles inside.
Natural environment described in step (a) refers under normal temperature and pressure, stands 4-8 hours in a natural environment, the filling perforation
Agent can solidify completely, play the effect for promoting ceramics strength after spackling solidification.
Using the lower surface of Sample A as viewing surface in step (b), it is placed on by Guangzhou Wei Yi metallographic test Instrument Ltd.
It is polished directly on the MP-1A type metallographic specimen polished machine of production, grinding and polishing parameter: revolving speed 800r/min;Hand-held grinding and polishing, pressure
It adjusts according to the actual situation, preferably pressure 0.5-2.0Kg, using water as lubricant.Grinding and polishing sand paper used is silicon carbide sand
Paper, the particle of the carborundum paper from thick to thin, first grind 3-10min with 800# sand paper;Change 1200# sand paper grinding 5-
10min;Finally use 2000# sand paper fine gtinding 10-20min.Until Sample A can be obviously observed under low power metallographic microscope
The interface of silicon-carbide particle.Porous ceramics metallographic specimen of the present invention is aobvious for metallographic in the preparation process of porous ceramics
Micro mirror observes the porous ceramics metallographic specimen internal structure, thus judge whether the quality of porous ceramics is good, it is highly beneficial
In the production cost for reducing the composite material or final products of preparing qualification using porous ceramics.
The present invention has especially selection to the aperture of porous ceramics and filler.In porous ceramic channel of the present invention
Corresponding filler is cooperated to make the porous ceramics of intensity difference and spackling compound within the scope of diameter, so that the metallographic examination of preparation
Sample has good abrasive characteristic, and will not destroy ceramic internal structure.Also pottery can be clearly observed under metallographic microscope
The size and distribution situation of porcelain internal particle.
Compared with the existing technology, beneficial effects of the present invention are as follows:
(1) preparation process of metallographic specimen of the present invention is simple, easy to accomplish without harsh preparation condition, preparation
Cost is very low.
(2) bad mechanical strength, not wear-resisting porous ceramics can be prepared into that mechanical strength is good, and wearability is good by the present invention
Metallographic specimen.
(3) metallographic specimen surfacing prepared by the present invention, inside metallographic microscope energy clear view metallographic specimen
Structure, applied to the quality testing in porous ceramics preparation process, being advantageous to, which reduces porous ceramics, prepares qualified answer
The production cost of condensation material or final products.
Detailed description of the invention
Fig. 1 is mold used in the present invention;Wherein 1 indicate mould sleeve, 2 indicate ceramics, and 3 indicate mold base.
Fig. 2 is the metallographic microscope of porous silicon carbide ceramic prepared by the embodiment of the present invention 2.
Fig. 3 is the metallographic microscope of porous silicon carbide ceramic prepared by comparative example 1.
Specific embodiment
In order to further allow the clear technical solution of the present invention of those skilled in the art, following embodiment is now enumerated
It is illustrated.It should be pointed out that following embodiment does not constitute a limitation effect to protection scope of the present invention.
Embodiment 1
A kind of preparation method of micrometer level porous ceramic metallographic specimen, comprising the following steps:
(a) taking a block size size is that 10mm × 10mm × 1mm porous silicon carbide ceramic is put into shown in Fig. 1 (1 in Fig. 1
Indicate mould sleeve, 2 indicate ceramics, 3 indicate mold bases) mold in, spackling, the filling perforation are then poured into mold
Agent is mainly made of epoxy resin and curing agent according to the ratio that mass ratio is 1:1, then stands 4 hours in a natural environment,
Sample A is made;
(b) Sample A is taken out, is polished directly, the micrometer level porous ceramic metallographic specimen is made.
The average pore size of the porous ceramics is 2 μm.
The spackling is liquid, the spackling leaving no air bubbles inside.
The process poured into described in step (a) is to pour into spackling along the upper surface of ceramics, up to spackling
Liquid level is higher than ceramics upper surface 4mm.Spackling is poured into along the upper surface of ceramics immerses shape in ceramic hole under the effect of gravity
At complex.
The curing agent is 650 Versamids, and the molecular weight of 650 Versamid is 600-1100.
Embodiment 2
A kind of preparation method of micrometer level porous ceramic metallographic specimen, comprising the following steps:
(a) taking a block size size is that 20mm × 20mm × 5mm porous silicon carbide ceramic is put into mold shown in FIG. 1
(1 indicates mould sleeve in Fig. 1, and 2 indicate ceramics, and 3 indicate mold base), then pours into spackling, the filling perforation into mold
Agent is mainly made of epoxy resin and curing agent according to the ratio that mass ratio is 2:1, and it is small then to stand 4-8 in a natural environment
When, Sample A is made;
(b) Sample A is taken out, is polished directly, the micrometer level porous ceramic metallographic specimen is made.
The average pore size of the porous ceramics is 15 μm.
The process poured into described in step (a) is to pour into spackling along the upper surface of ceramics, up to spackling
Liquid level is higher than ceramics upper surface 5mm.Spackling is poured into along the upper surface of ceramics immerses shape in ceramic hole under the effect of gravity
At complex.
The spackling is liquid, the spackling leaving no air bubbles inside.
The epoxy resin is bisphenol A type epoxy resin.
The curing agent is 650 Versamids, and the molecular weight of 650 Versamid is 600-1100.
Fig. 2 is the micrometer level porous ceramic metallographic specimen that embodiment 2 is prepared, and grinding effect is preferable, and metallographic specimen is not
Picking phenomenon occurs, the distribution of size particles can be observed.Further, since abradant surface is just very smooth, picture clarity
It is higher.Grey polygon substance is the grain section of porous silicon carbide ceramic in Fig. 2, and black portions are spackling.Grey in Fig. 2
The distribution situation of substance is able to reflect out the distribution characteristics of porous ceramic particles, by whether having tiny in observation metallographic specimen
The reunion of grain, and the quantity of silicon-carbide particle in multiple visual fields is counted to assess the even particle distribution of porous silicon carbide ceramic
Property.
Embodiment 3
A kind of preparation method of micrometer level porous ceramic metallographic specimen, comprising the following steps:
(a) taking a block size size is that 20mm × 20mm × 3mm porous silicon carbide ceramic is put into mold shown in FIG. 1
(1 indicates mould sleeve in Fig. 1, and 2 indicate ceramics, and 3 indicate mold base), then pours into spackling, the filling perforation into mold
Agent is mainly made of epoxy resin and curing agent according to the ratio that mass ratio is 1-3:1, and it is small then to stand 5 in a natural environment
When, Sample A is made;
(b) Sample A is taken out, is polished directly, the micrometer level porous ceramic metallographic specimen is made.
The average pore size of the porous ceramics is 12 μm.
The process poured into described in step (a) is to pour into spackling along the upper surface of ceramics, up to spackling
Liquid level is higher than ceramics upper surface 8mm.Spackling is poured into along the upper surface of ceramics immerses shape in ceramic hole under the effect of gravity
At complex.
The spackling is liquid, the spackling leaving no air bubbles inside.
The epoxy resin is bisphenol A type epoxy resin.
The curing agent is 650 Versamids, and the molecular weight of 650 Versamid is 600-1100.
Embodiment 4
A kind of preparation method of micrometer level porous ceramic metallographic specimen, comprising the following steps:
(a) taking a block size size is that 30mm × 30mm × 5mm porous silicon carbide ceramic is put into mold shown in FIG. 1
(1 indicates mould sleeve in Fig. 1, and 2 indicate ceramics, and 3 indicate mold base), then pours into spackling, the filling perforation into mold
Agent is mainly made of epoxy resin and curing agent according to the ratio that mass ratio is 3:1, then stands 8 hours in a natural environment,
Sample A is made;
(b) Sample A is taken out, is polished directly, the micrometer level porous ceramic metallographic specimen is made.
The average pore size of the porous ceramics is 20 μm.
The process poured into described in step (a) is to pour into spackling along the upper surface of ceramics, up to spackling
Liquid level is higher than ceramics upper surface 10mm.Spackling is poured into along the upper surface of ceramics immerses shape in ceramic hole under the effect of gravity
At complex.
The curing agent is 650 Versamids, and the molecular weight of 650 Versamid is 600-1100.
Comparative example 1
The size that the sample of comparative example 1 directly cuts porous silicon carbide ceramic is 20mm × 20mm × 15mm, then
Carry out grinding observation.Fig. 3 is the metallographic microscope of the porous silicon carbide ceramic of comparative example 1.The metallographic of comparative example 1 as can be seen from Figure 3
Sample picking is serious.Observe that metallographic specimen surface little particle is still covered on large particle surface, Wu Faguan with metallographic microscope
Bulky grain is observed, can not also observe the situation inside metallographic specimen.
Product measure of merit
Product and commercially available similar-type products prepared by Example 1-4 and comparative example 1, is tested bending strength (MPa)
(testing standard of bending strength is GB/T4741-1999 " ceramic material anti-reflecting bending strength test method ") and wearability are (in 0.5Kg
It is detected under conditions of pressure, 1000 mesh diamond sand paper, speed of grinding plate 500r/min, milling time 30s, wet friction wear-resisting
Property), control sample the thickness of sample reduction and is recorded before and after undergoing wearability test, and the results are shown in Table 1.
Table 1:
As can be seen from Table 1, the bending strength and wearability of the product of embodiment 1-4 preparation of the present invention are obvious
It is got well than the bending strength and wearability of product and commercially available similar-type products prepared by comparative example 1.Moreover, from embodiment 1-4
The experimental data of the product of product and comparative example 1 preparation of preparation, which can be seen that spackling of the present invention, significantly to be played
Improve the effect of the bending strength and wearability of product.In addition being averaged for porous silicon carbide ceramic selected by the present invention is also indicated that
Aperture also has particularity.
In addition, the metallographic specimen also prepared to embodiment 2 and comparative example 1 has carried out metallographic microscope observation experiment, Fig. 2 is
The metallographic microscope of porous silicon carbide ceramic prepared by the embodiment of the present invention 2.Fig. 3 is porous silicon carbide ceramic prepared by comparative example 1
Metallographic microscope.The phenomenon that loses powder does not occur for metallographic specimen as can be seen from Figure 2, and the distribution of size particles can be observed.In addition, by
Just very smooth in abradant surface, picture clarity is higher.The metallographic specimen picking that as can be seen from Figure 3 prepared by comparative example 1 is serious.
It observes that metallographic specimen surface little particle is still covered on large particle surface with metallographic microscope, can not observe bulky grain,
The situation inside metallographic specimen can not be obviously observed.
Claims (10)
1. a kind of preparation method of micrometer level porous ceramic metallographic specimen, which comprises the following steps:
(a) porous ceramics is put into mold, then pours into spackling into mold, the spackling mainly by epoxy resin and
Curing agent is formed according to the ratio that mass ratio is 1-3:1, is then allowed to stand 4-8 hours, and Sample A is made;
(b) Sample A is taken out, is polished directly, the micrometer level porous ceramic metallographic specimen is made.
2. preparation method according to claim 1, which is characterized in that the porous ceramics is porous silicon carbide ceramic.
3. preparation method according to claim 1, which is characterized in that the average pore size of the porous ceramics is 2-20 μm.
4. preparation method according to claim 1, which is characterized in that the size of porous ceramics described in step (a)
For 10-30mm × 10-30mm × 1-5mm;The mold includes mould sleeve (1), mold base (3).
5. preparation method according to claim 1, which is characterized in that the process poured into described in step (a) is that will fill out
Hole agent is poured into along the upper surface of porous ceramics, until the liquid level of spackling is higher than porous ceramics upper surface 4-10mm.
6. preparation method according to claim 1, which is characterized in that the epoxide number of the epoxy resin is 0.41-
0.47mol/100g。
7. preparation method according to claim 1, which is characterized in that the curing agent is epoxy curing agent.
8. preparation method according to claim 7, which is characterized in that the epoxy curing agent is low molecule polyamides
Amine, the molecular weight of the Versamid are 600-1100.
9. a kind of micrometer level porous ceramic metallographic specimen, which is characterized in that the micrometer level porous ceramic metallographic specimen is by right
It is required that preparation method described in any one of 1-8 is prepared.
10. a kind of application of micrometer level porous ceramic metallographic specimen according to claim 9, which is characterized in that will be described
Micrometer level porous ceramics metallographic specimen is applied to micrometer level porous ceramic internal structure described in metallography microscope sem observation.
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