Open tender conditions
Annex 4

Technical specification

Medium resolution scanning electron microscope (SEM)

Prepared by j.m.d. Martynas Lelis

General description:

Equipment is designated for the analysis (surface and cross sections) of metal hydrides used for hydrogen storage, various oxides used for fuel cells and gas purification membranes. The SEM should be suitable to both for analysis of thin films and powder material. The equipment will be mainly used for the collection of fundamental information about structure of investigated sample (surface and cross section), morphology, existence of defects and their structure etc.

Note:For the standards, particular processes, trademarks and certificates which are described in this specification supplier can provide equivalent solutions.

No. / Technical parameter / Requirement for technical parameter
1 / Secondary electron (SE) resolution /
  • Not worse than 3 nm at high vacuum and 30 kV acc. voltage;
  • Not worse than 10 nm, at high vacuum and 3 kV acc. voltage.

2 / Backscattered electron (BSE) resolution /
  • Not worse than 4 nm at high and low vacuum and 30 kV acc. voltage.

3 / Magnification /
  • In the case then SEM manufacturer judges magnification in accordance to displaying image on standard Polaroid image size the magnification should cover at least the range of 5x - 300 000x;
  • In the case then SEM manufacturer judges magnification in accordance to displaying image on standard 19” size LCD display the magnification should cover at least the range of 15x – 1 000 000x;
  • In the case then SEM manufacturer judges magnification in accordance to displaying image on any other object/size, then corresponding recalculated magnification should satisfy at least one of the above mentioned requirements.

4 / Electron optics /
  • Continuously adjusted beam current at least up to 1 μA;
  • The lowest value of feasible acceleration voltage must be not higher than 300 V; the highest value of feasible acceleration voltage must be not lower than 30 kV; i.e. SEM must cover be at least 0,3-30 kV minimal interval;
  • Requested analytical working distance: WD = 10±5 mm.

5 / Detectors /
  • The supplied SEM must have proper set of detectors to be able to make decent SE and BSE measurements under all conditions which are declared by this technical specification including high vacuum and low vacuum (unless exception are foreseen by separate clause).
  • The used set of detectors must warrant that requested SE and BSE image resolution will be achieved under both high and low vacuum and corresponding acceleration voltage values conditions;
  • The SE detector for high vacuum operation must be of Everhardt Thornley type;
  • Working at low vacuum regime one or several specially designated high tech SE detectors must be used. This detector (or detectors) must cover whole pressure range foreseen in issue No. 6 of this specification, the detector (or detectors) must be suitable to work under any pressure from the later range.
  • Separate BSE detector (or set of BSE detectors) for high and low vacuum regimes;
  • BSE detector which is designated to work at high vacuum conditions must have at least 4 segments and at least three different working regimes: where one must be designated to stress surface topography and another one must stress elemental composition differences;
  • All supplied detectors must be delivered together with all hardware (for example detector amplifier) and software which are necessary for their required functionality.
  • Montage angle of EDS detector must be 35 degree and it must be possible to perform EDS analysis at both high and low vacuum conditions.
  • SEM must be supplied with suitable IR-CCD camera for real time large scale sample display and fast finding of analysis point.

6 / Vacuum system /
  • SEM must have fully automated control system (of vacuum pumps and valves) to perform automatic pumping and venting procedures;
  • SEM must have at least one high vacuum mode and at least one low vacuum mode;
  • At high vacuum measuring mode it should be possible to achieve at least 1,5 x 10-3 Pa vacuum level;
  • At low vacuum mode pressure in sample chamber bust be controlled at least in the interval of 10-270 Pa;
  • All vacuum pump system, including high vacuum and forevacuum pumps must be oil-free. Usage of oil filters and traps in the system is not treated as proper alternative;
  • To achieve adequate pumping time vacuum system must be employed with powerful high vacuum pump: if vacuum system uses turbo molecular pump (TMP) it should be of not less than 200 L/s pumping speed; if other type of high vacuum pump is used that its effective pumping power should be not less than that of 200 L/s TMP pump.
  • To achieve adequate pumping time vacuum system must be employed with powerful forevacuum pump: the oil free forevacuum pump must be of optimal pumping power but not less than 120 L/min;
  • The forevacuum pump or pumps which are used with SEM must be supplied with appropriate acoustic enclosure which has own ventilation and overheating security alarm (beep or other sound);
  • Sensible full range vacuum gauge or set of gauges for SEM security system to stop operation if leaking or vacuum failure error appears.

7 / Sample stage /
  • Fully motorised 5-axis computer controlled eucentric sample stage;
  • Minimal range of movement in X axis: 100 mm;
  • Minimal range of movement in Y axis: 50 mm;
  • Minimal range of movement in Z axis: 60 mm;
  • Minimal requirement for sample tilt T: from at least -5° up to not less than +70°;
  • Rotation R range: continuous/not limited 360° rotation.

8 / Control of SEM /
  • SEM must be fully operated by personal computer (PC) which has MS windows XP or newer MS Windows operation system with appropriate SEM control software including image saving and processing software. Also the supplied computer must have MS Office software package;
  • Support PC for installation of user programs, data storage and connection to internet, connected to main control PC. It must to be possible to control both PC (main and support) by single mouse and keyboard; i.e. SEM must be supplied with appropriate hardware and software for one keyboard and one mouse control on two computers;
  • At least two not smaller than 19” LCD monitors for easy and comfortable operation of computers and software;
  • Obligatory control accessories:
a)manual user interface where main SEM working parameters (focus, magnification, stigmatism, brightness, contrast etc.) are controlled by convenient knobs and buttons;
b)manual sample position manipulation unit: joystick or trackball.
9 / Image registration, display and processing /
  • Full screen image of not less then 1280x960 pixels;
  • Hardware and software must allow simultaneously display at least two images based on different detectors;
  • SEM must have option to choose from several scan speeds including real time (“live”) image display;
  • Possibility to save different resolution images;
  • Maximal horizontal resolution not less then 4000 pixels and maximal vertical resolution not less than 3500 pixels;
  • Possibility to choose image saving format with JPEG, TIFF and BMP are obligatory options. AVI video formation option would be beneficial;
  • SEM must have up-to-date technology software for recorded data (images) management with obligatory image post processingpossibility;
  • SEM must be employed with appropriate hardware and software for 3D image formation. 3D image can be formulated based on photogrammetry (3D image is formulated from two or more images recorded at different tilt angles) or photometric stereo (3D image is formatted by using images recorded by different segments of BSE detector) method. Minimal requirements for 3D software: 3D image formation for intuitive visualisation (close up, increase viewing distance, changing angle etc.), surface roughness parameters measurements, display of selected line profile, automatic calibration function, coloured relief representation, 3D image storage and opening of saved data;
  • Software for equipment operation and data analysis must be installed in the provided computer and additionally supplied in CD or DVD hardcopy.

10 / Sample holders /
  • 50 units of flat top surface sample holders compatible with delivered SEM where diameter of sample stage must be of 12.5±2.5 mm. Bellow in this specification this type of sample holders will be designated as BL1;
  • 10 units of flat top surface sample holders compatible with delivered SEM where diameter of sample stage must be of 25±2 mm.
  • 2 units of flat top surface sample holders compatible with delivered SEM where diameter of sample stage must be of 50±5 mm.
  • 1 unit of flat top surface sample holder compatible with delivered SEM where diameter of sample stage must be of 95±5 mm.
  • 1 unit of flat, compact variable tilt specimen mount (angle changing in at least 0° – 90° interval with markings for 30°, 45°, 70° and 90°) with not smaller than 10x10mm sample table size;
  • 1 unit of specimen holder for 4 sample holders of type BL1;
  • 1 unit of 45° pre-tilt holder for BL1 type sample holder;
  • 1 unit of split mount specimen holder for thin samples (metals, ceramics, plastics etc.) cross section measurements where maximal size of suitable samples must be at least 6 mm;
  • 1 unit of set screw vise sample holder with not smaller than 4 mm opening slot designated for thin sample cross section with sample fixing with screw from the side;
  • 1 unit of double slotted vise sample holders with not smaller than 1 mm opening slots designated for thin sample cross section with sample fixing with screw from the side;
  • 1 unit of tube/needle clamp for examining wire cross sections or needle tips with diameter of at least 2mm;
  • 5 units of BL1 type sample holders for holding flat or thin specimens (such as 7x7 mm Si chips) with sample fixing with a small screw (desirably with a small clamp) at the side of the sample holder;
  • 1 unit of variable angle (from 0° up to 180°) cross section sample holder for samples with up to at least 6 mm thickness;
  • 1 unit of double slotted vise sample holders with 2.5±0.5 mm opening slots designated for thin sample cross section with sample fixing with screw from the side;
  • 1 unit of specimen holder for 8 sample holders of type BL1;
  • 1 unit of four standard geological thin sections or slides (or other similar size samples) of at least up to 47 x 27 mm size, thickness up to 3 mm.
  • 1 unit of universal sample holder, where sample is pressed by two springloaded plates. Plates must have special slots to firmly hold round samples of various diameters both horizontally and vertically. Maximal achievable distance between plates must be not less than 35 mm;
  • 1 unit of universal large bulk specimen holder holds larger irregular and round specimens fixed with at least four side screws and holds up to at least a diameter of 50 mm;
  • All of the above mentioned sample holders must be produced from materials which are fully compatible with environment which is present in SEM: vacuum, Electron beam etc. Also, sample holders should not be produced from materials which could inadequately disturb primary or SE/BSE electrons;
  • All of the sample holder must supplied in the corresponding carriage boxes made from wood, plastic or metal. The amount and size of these boxes should be enough to comfortably place all of the mentioned sample holders without them touching each other;
  • 1 unit of special specimen mount gripper for standard size (BL1 type 12,5±2,5 mm diameter) sample holder and 1 unit of special specimen mount gripper for medium size (25±2 mm diameter) sample holder;
  • 500 units of 6±1 mm diameter carbon conductive tabs suitable for sample mounting onto sample holder;
  • 500 units of 13±2 mm diameter carbon conductive tabs suitable for sample mounting onto sample holder;
  • 30 g of Ag based conductive paint which would be suitable for sticking of conductive and non-conductive sample to sample mounts and charge grounding. They also should have good “metal to metal” adhesion properties;
  • 100 g carbon based conductive paint (water or alcohol based) which would be suitable for sticking of conductive and non-conductive sample to sample mounts and charge grounding especially in place there Ag based paint is not suitable (for example EDS analysis).

11 / Obligatory accessories /
  • Equipment maintenance and cleaning kit must include:
  • aset of spare parts and consumables (filaments, apertures, etc.) whose average declared working resource is shorter than 2 years (estimating average usage of 7 hours per working day and 5 working days per week). The provided amount of each type of consumables must be enough for 2 years of average usage (according to manufacturer declaration) but must be not less than 40 units of W filaments (if SEM uses LaB6 filaments then minimal amount is 5 units) and at least 5 apertures (if they are changeable).
  • at least 100 units of special cleaning/polishing tissues and at least 150 g of special paste for the gentle cleaning/polishing of sensitive metallic SEM parts (such as wehnelt);
  • If standard maintenance procedures of supplied oil-free pump requires to perform periodic change of pumps O-rings or other parts whose maintenance interval is shorter than 2 year, then supplier together with supplied equipment must deliver at least one complete set of replaceable parts. As an alternative supplier can commit himself to perform all maintenance including change of consumable parts (which is foreseen by pump manufacturer at its user manual) of the supplied oil-free pump for two year period;
  • If SEM uses water for cooling, then appropriate water cooler must be supplied together with the instrument;
  • Dehumidifier for the foreseen room of the exploitation must be included in the proposal. Minimal output requirement for dehumidifier is at least 26 l/24h (at 30 °C and 80% humidity), but maximal serviceable volume of the room which is declared by the dehumidifier manufacturer must be not less than the volume of real foreseen room, i.e not less than 180 m3;
  • For the safe operation of SEM and all of its auxiliary systems including vacuum pumps, computers, EDS analysis system, laser printer the system must be supplied with single phase “on-line” type UPS power source of not less than 8 kW (11 kVA) peak power and at least 3 min of backup power energy under 100 % (8kW) load;
  • special calibration sample for the calibration of EDS energy and BSE detector response curve using different mass elements. Calibration sample must have at least 10 different elements whose atomic numbers are gradually spread in the range from of Z=6 up to Z=85±5. Necessary elements are C and Si. Additionally this calibration sample must have 200±50μm diameter hole. Delivered calibration sample must be mounted on the appropriate sample holder which is compatible with the delivered SEM or it must have appropriate conversion joint.
  • Special durable calibration sample for the calibration of SEM magnification and scale. Calibration sample must have at least 4 different calibration size features, with the smallest one being not larger than 100 nm and the biggest one not smaller than 0,5 mm. This calibration sample also must have sufficient contrast for the SE and BSE electrons and suffer from charging effects. The sample also must have NIST (or equivalent) certificate or must be traceable up to according NIST standard (or equivalent).

12 / Other requirements /
  • Lithuanian energy institute owns EDS system and wants it to be installed in the supplied equipment, therefore supplied equipment must be fully compatible with Bruker Quad 5040 EDS chemical microanalysis detector and its software Quantax 800; i.e. there must be no technical limitations to install Bruker Quad 5040 EDS into the supplied SEM equipment and to keep all functionality of Bruker Quad 5040 detector which is declared by its manufacturer.
  • During installation of the supplied SEM supplier also must fulfil following actions:
  • During equipment installation supplier have to observe the functionality of JEOL JSM-5600 electron microscope and Bruker Quad 5040 EDS system which is installed at it. During observation supplier must document the fact of the instruments functionality or not functionality and to document main parameters describing instrument functionality (resolution, EDS energetic throughput etc.);
  • To take out Bruker Quad 5040 EDS system (detector and its accessories if they are present) from the JEOL JSM-5600 SEM;
  • The taken off EDS system must be installed into the supplied SEM;
  • After the detector is taken from JEOL JSM-5600 supplier must fix up old JEOL JSM-5600 SEM: i.e. supplier must mount the original cover which was removed during EDS installation (the cover is not harmed and is stored at LEI) and perform all other actions or changes which are needed to return JEOL JSM-5600 into the functionality state which was documented before EDS being taken out of it;
  • If after EDSplacement from JEOL JSM-5600 to the supplied SEM any of the concerned equipment (supplied SEM, JEOL JSM-5600 and Bruker Quad 5040 EDS) becomes unfunctional or does not reach the parameters which are required by this technical specification the supplier must fix the observed problems for equipment to be fully functional or must prove that losing of functionality has arisen not due to his (or his representatives) fault;
  • All expenses including but not limiting labour and needed supplies, which are related to the detectors disassembling from old microscope and installation to the supplied SEM as well as restoring of functionality of all three instruments (under condition which are foreseen in this specification) has to be covered by the supplier therefore they must be included in the proposal price.

13 / Acceptation tests /
  • Equipment acceptation tests (conformance to this technical specification) must be performed after its installation at permanent usage place – Kaunas, Lithuanian Energy Institute.

14 / Warranty conditions /
  • The supplier must warranty that at the moment of SEM installation it has no visible or covered defects related inappropriate construction and instrument design, used materials and human factor;
  • If any of such defects are observed during 24 months after instrument acceptance tests and acceptance signing date, the supplier shall change parts or otherwise fix all of the observed defects:
  • If defects are observed during warranty period and for their fixing supplier or its representatives uses used spare parts or components, then all of them must be provided with not shorter than 6 months warranty (starting from the day of defect elimination) or till the end of initial warranty period whichever is longer;
  • If defects are observed during warranty period and for their fixing supplier or its representative uses only new parts or components, then all of them must be provided with warranty which validity is not shorter than the end of the main warranty.

15 / Installation /
  • Supplier must cover all expenses related to the equipment assembly and installation at its exploitation place (including transfer of the existing Bruker Quad 5040 EDS microanalysis system from old JEOL JSM-5600 microscope to the delivered SEM). Delivery costs as well as custom duties (if they are aplliecable) also must be covered by the supplier therefore all these costs has to be included in the proposal.

16 / Training /
  • Supplier must perform introduction training of equipments usage at Lithuanian Energy Institute facility after unit installation and this must be included in the proposal price. The netto time of introduction training must be not shorter than 4 hours and equipments installation, testing and conformance to technical specification can not be included into these 4 hours of training time.

17 / Documentation /
  • Equipment must be supplied with at least one manual in english describing how to use all parts of the instrument and how to make its maintenance.

18 / Service /
  • If problems with delivered equipment arise or it shows any kind of malfunctioning the supplier must respond within 48 hours after the announcement of the observed problem (considering that announcement is being made in working days (Monday-Friday) from 8 a.m. till 5 p.m.

19 / Quality assurance /
  • Equipment and its parts must be manufactured in accordance to ISO 9001 or equivalent quality assurance requirements.

______