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Metallographic sample preparation report of Mo-TiC20%

2022-03-14

Molybdenum is a refractory metal, which has the characteristics of high melting point, high temperature strength, good thermal conductivity and electrical conductivity, low thermal expansion coefficient, resistance to corrosion by molten salts and liquid light metals. Molybdenum and its alloys are commonly used in powder metallurgy processes. Molybdenum powders doped with specific elements and compounds can be pressed and sintered to form high-strength metal products.



01Equipment and consumables

Equipment

Trojan Alpha-600 automatic grinder&polisher;

Trojan FlexPRESS mounting press;

Leica DM2700M metallographic microscope;

Hairdryer;

Consumables

Degreasing cotton;
Trojan TJ2237 edge retention epoxy resin
;
Trojan PL-W polishing lubricant
;
Trojan diamond disc(P120
;P400;P1500);
Trojan YS-JP white fiber polishing cloth(8in)
;
Trojan ZN-JP black polyurethane polishing cloth(8in)
;
Trojan 3
μm polycrystalline diamond suspension ;
Trojan 0.05
μm non-crystallizing silica.


02 Sample preparation procedure

1-Mounting

After ultrasonic cleaning of the specimens, hot mounting the specimen with FlexPRESS mounting press.


FlexPRESS mounting press


Equipment

FlexPRESS mounting press

Consumables

TJ2237 edge retention epoxy resin

Parameter

180℃,160Bar,4min,medium speed cooling

2- Grinding

Polish the specimen with Alpha -600 automatic grinder&polisher, diamond grinding disc P120→P1500.


Alpha-600 automatic grinder&polisher


Diamond grinding disc

Equipment

Alpha-600 automatic grinder&polisher

Consumables

Diamond grinding disc:P120,P400,P1500

Parameter

Upper disc:100rpm,lower disc:300rpm,same direction,pressure:25N

3.1-Polishing(plane polishing)

Polish the specimen with Alpha-600 automatic grinder&polisher,use YS polishing cloth with 3μm polycrystalline diamond suspension for plane polishing. Note that PL-W polishing lubricant should be added for polishing.


YS-JP white fiber polishing cloth

Diamond suspension

Equipment

Alpha-600 automatic grinder&polisher

Consumables

YS polishing cloth,3μm polycrystalline diamond suspension,PL-Wpolishing lubricant

Parameter

Upper disc:100rpm,lower disc:150rpm,reverse direction,pressure:25N,time:10min

3.2-polishing(fine polishing)

Polish the specimen with Alpha-600 automatic grinder&polisher,use ZN polishing cloth with 0.05μm non-crystallizing silica suspension for fine polishing.(add 3% hydrogen peroxide in non-crystallizing silica suspension)


ZN-ZP black polyurethane polishing cloth


Non-crystallizing silica suspension

Equipment

Alpha-600 automatic grinder&polisher

Consumables

ZN-ZP black polyurethane polishing cloth,0.05μm non-crystallizing silica suspension(add 30% hydrogen peroxide)

Parameter

Upper disc:100rpm,lower disc:120rpm,same direction,pressure:20N,time :5~10min

4- Corrosion

After 10min polishing with non-crystallizing silica suspension, The general outline of each phase in the sample has been revealed (see the figure below),Just need to corrode a little.


After polishing with silica 500×

The boundaries are clearly visible

Reagent

15% potassium ferricyanide and 15% sodium hydroxide aqueous solution are mixed in a ratio of 2:1

Instructions

Abrasion method, time:5~10s

5-Observation


Equipment

MN 60 series microscope

Parameter

50×→500×

03 Analysis

Mo-TiC 500×


Mo-TiC 500×

Visible light blue TiC, black holes, white molybdenum and other equiaxed grains


Mo is a hard and tough metal. In this example, Mo and TiC are sintered, and the hardness of TiC is about 3400HV, which is much higher than 2550HV of SiC. Therefore, SiC sandpaper should not be used for grinding this metal. It should be replaced with diamond grinding disc.

Plane polishing is relatively simple, use a hard woven cloth with polycrystalline diamond suspension.

During fine polishing, use a soft damped polishing cloth for chemical mechanical polishing to release the stress on the surface of the sample, and pay attention to controlling the time to avoid too much embossing for phases with different hardnesses.

After silica polishing, since the stress on the surface of the sample is released to a large extent, the subsequent etching becomes extremely simple, and the etchant can be used to slightly rub for a few seconds. Pay attention to protection, the corrosive liquid is poisonous!

In the metallographic phase, the light blue is TiC, the black is the hole, and the white is the molybdenum equiaxed grain. The dark area around TiC should be the diffusion and fusion area of TiC and Mo.

Referring to GB-T 41080-2021 "Molybdenum and molybdenum alloy metallographic examination methods" 9.2 grain assessment of 9.2.1 appendix B of the comparative method, the grain size of molybdenum is at or better than M10 grade.
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