Metallurgical Lab from 0s 4

[GTLA]

Did someone have developed a metallurgical laboratory from nothing? I am working on that, our business is considering this and im who will justify the cost. I have visited some suppliers and determined what we need based in current external analysis; by now I have included stereomicroscope & metallurgical microscope (Nikon), hardness & microhardness testers (Instron), cutting-mounting pulisher (Struers), EDS (Spectro) and SEM (Jeol, but i guess maybe this will be included later). I though this will be enough to conduct good analysis in our parts, we handle metallic and plastic parts for safety systems.
Any tip or experience that you may have on it? I would like to ensure that i am not missing something. Thanks.

 

[TVP]

Does your company already have a universal test machine, also known as a tensile tester? Will you be required to test for mechanical properties (yield strength, tensile strength, elongation)? What about chemical composition determination? I would recommend that you outsource this unless you will be doing it everyday, because it requires a lot of calibration on top of the already considerable cost of the equipment. Have you included digital cameras and software for the cameras to be used with the microscopes? This is extremely important for creating useful reports, and for archival purposes. You may want to consider an enterprise system such as Scentis from Struers. Image analysis is another software package that is usually separate from that for operating the camera. Clemex makes a very good package. The last items are the consumables (resin for mounting, grinding & polishing cloths and abrasives), glassware (beakers, dishes, etc.), and similar everyday lab items.

 

[GTLA]

Yes, we already have 2 universal testers. We just dont have the clamps, but they are already considered. For the chemical analysis, i was considering the EDS from Broker and Spectro; according them, these do not needs calibration just some easy "adjustments", i have quoted and with 70 outsource analysis we may pay an own equipment.
Cameras and software is already considered too, Zeiss includes a software that may put all the metallography in a report but i will ask for a Scentis demo too.
Thanks for the support.

 

[CoryPad]

I have created a metallurgical laboratory from nothing. In addition to the universal testing machine, cameras, software, consumables, and glassware TVP mentioned, you probably will need (or have access to) sample preparation equipment like saws, shear, grinder, lathe, mill; a full toolbox, measurement equipment (calipers, micrometers, ultrasonic thickness gauge, coating thickness gauge), and environmental chambers (corrosion, humidity, temperature). If you are doing metal impact, then maybe a Charpy or an instrumented impact machine. If you are doing polymer analysis, then you probably will need an FTIR, DSC, TGA, HDT, and Izod impact tester.

 

[GTLA]

Right!, just are missing to add the thickness gauges.
We are not requiring that measurements to frequent but i will review costs, maybe is shipper to buy the equipment than some services.
Not metal impact in the scope neither polymer analysis (by now).

 

[CoryPad]

A few more things:

high-purity water source (reverse osmosis is common)

spatulas, spoons, stirrers, etc. (metal, plastic, glass)

balances: low mass (~ 500 g), high precision one for making solutions; a medium sized one (~ 5 kg) for measuring part mass or water for solutions; a high mass one (~ 50 kg) for heavy parts, salt for corrosion testing, etc.

furnace (temperature > 1000 [°]C) for heat treating, coating removal, etc.

hot plate, ultrasonic cleaner

fume hood to work under

 

[arunmrao]

A good library,with reference standards,reference micrographs,handbooks,basic text books, will be useful.




If you think education is expensive, try Ignorance.
- Andy McIntyre


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[dbooker630]

You will also need a spill control kit in case of an acid spill; an eye wash, and shower. Accidents can happen.

 

[CoryPad]

Good advice from dbooker630.

Another item - dessicator to prevent oxidation of metallographic specimens.

You may not need one, but a small vacuum pump is great for preparing cold mounted (usually epoxy) specimens.

 

[GTLA]

Good advices, thanks to all for your comments.
Im already considering all of them.

In the elemental analysis, did you have worked with Mg samples? Do you know if same result is get for it with EDS system and atomic absorption method? I have alloys where Mg is aroung 98% of them. I heard that EDS is not accurate for Mg, but suppliers told me that the current equipments does not have issue with that and readings may be done with the corresponding module.

 

[CoryPad]

EDS can detect Mg, but you can't use EDS for definitive composition of any alloy.

The quantitative analysis of Mg that I was a part of used ICP.

 

[TVP]

GTLA,

As I mentioned previously and CoryPad just confirmed, you cannot use EDS to "certify" the chemical composition of an item. EDS is capable of semi-quantitative chemical analysis, which means that you can determine whether or not it is an iron-based alloy with some additions of Cr & Mo, but you cannot certify that it is alloy 4130 (UNS G41300) according to SAE J404. This requires a quantitative method such as ICP-AES, ICP-AA, OES, etc. With regards to Mg sensitivity, all new EDS systems are capable of resolving low atomic mass elements like Mg-- previously there were limitations, but now they can detect at least down to B, maybe Be or Li.

 

[salmon2]

Then it can detect C, which is most important for carbon steel?

 

[tripleZ]

How accurately can the new EDS systems gage Boron content? Meaning, does the boron content have to be of a certain % of the total material to adequately pick it up? Or are trace amounts (say in the .025% range) able to be detected?

Sorry for the hijack. We've just never been able to get a good B trace estimation with the company we currently use for EDS.

 

[CoryPad]

salmon2,

An EDS can detect carbon, but it cannot provide the proper accuracy for carbon determination in steels. In fact, carbon and oxygen peaks are present for almost any specimen put into an electron microscope chamber and usually ignored.

tripleZ,

Boron is added to steel at a concentration of 0.0005 to 0.003 mass percent. At this concentration, the best way to detect boron is to use a silicon drift detector that can sample at 500,000 counts per second, which is enough to get a boron signal in a reasonable amount of time.

 

[TVP]

tripleZ,

Corypad probably should have clarified that these silicon drift detectors have only become commercially available in the past 5 years or so, meaning that many test facilities have EDS systems older than this, hence the poor B determination. You should specifically talk to the EDS operator at your vendor and ask if they have a silicon drift detector. Bruker is one supplier of this type of system:

http://www.bruker-axs.de/xflashsddx-raydet0.html

 

[GTLA]

What is the main difference in the results get with an EDS (optical system) and an EDX (x-ray)? I mean, they give you similar reads, but reading different energies. Are the results the same?

In the other hand, i already have some quotes for the SEMs. I'm really interested in the Zeiss EVO-MA and the FEI Phenom (cost is almost the halpf than the Zeiss). Potence is so different, but 20,000 in the FEI is enough for morphologycal analysis in metal. Am I right??? What about the performance of these equipments? does anyone have worked with them?
Sorry for to many questions, but i am relatively new in this field. Thanks.

 

[CoryPad]

You need to educate yourself on elemental analysis techniques and equipment. The words "EDS (optical system)" is gibberish.

I can attest that the Zeiss EVO MA is an excellent microscope that can fulfill almost any type of work.

The FEI Phenom is an example of a newer tabletop SEM with reduced capabilities (and reduced price!). If you are interested in this, you should cross-shop with the Hitachi TM-1000 and the Nikon/JEOL NeoScope:

http://www.hitachi-hta.com/pageloader~type~product~id~450~orgid~42.html

http://www.jeolusa.com/PRODUCTS/Ele...um/NeoScopeBenchtopSEM/tabid/511/Default.aspx

 

[GTLA]

Well, maybe i make the question confusing.
I know that EDS is that, but i was referring about 2 different equipments. I have knew one that conduct the analysis measuring the light's wave length and relating it with the element (that's why a said optical). And the most common (at least is the one that i knew before) is which measure the x-rays emmited by electrons movement. Anyway thanks for your answer.

 

[DABwilldo]

I've set up X-ray spectrometers in several steel mills over the years. (I used to work for Philips) The mills I worked with used Wavelength Dispersive X-ray Fluorescence Spectrometry (WD-XRF) or Optical Emmission Spectrometry (OES) for quality control. Elements lighter than Na are handled by OES or other analytical tools. (LECO Carbon analyzer, for example)

Energy Dispersive X-ray Fluorescence Spectrometry (EDS-XRF) can provide quanititative results on elements heavier than Na and present in concentrations greater than 1000ppm, generally speaking. You need reference standards of the same alloy to compare to. Quantitative analyses of unknowns, without appropriate reference standards is not practical.

WD-XRF can provide quantitative results on a wide range of alloys for elements heavier than Fluorine, for concentrations ranging from 10ppm up to 99 wt%. There are a few elements that have lower, and still accurate limits of quantification, but they require specific hardware inside the instrument. The details are too involved for the purposes of this discussion.

The main problem with X-ray analysis of low Z elements in steel is that the signal to noise ratio is poor. The iron matrix blots out the signal from the elements like Oxygen, B and Carbon. The signal from these elements is also measured from only the very surface of the specimen, and so surface finish and preparation become extremely important. Small changes in surface prep can destroy your accuracy.

In general I would characterize X-ray Fluorescence analysis as a poor tool for quantitative analysis of low Z elements in steel.

I do not know as much about OES as I do about XRF. I do know that OES has much better capability for some low Z elements. We analyze for B in steel using our OES in-house and appear to have very low limits of quantification; on the order of 0.1ppm. This is anecdotal, as I didn't set up the equipment. I just see the results cross my desk.

So, for an analytical lab, I wouldn't rely on EDS-XRF in your electron microscope for defensible quantitative analyses. You'll need some other tools if this is a capability that you must have in house. You can cover a lot of analytical ground with a WD-XRF or an OES. I believe that the WD-XRF will handle a wider variety of materials than an OES; like liquids, slurries, powders, and non-conductive materials. So if flexibility is important, you might look at WD-XRF.

The specimen prep for WD-XRF can be less labor intensive than either AA or ICP. It has the added benefit of being more or less non-destructive.

There are WD-XRF modules for SEMs. But all the WD-XRF equipment is costly, when compared to AA or EDS-XRF systems. It's a situation where, "you get what you pay for".

Hope this helps...