Osmium Plasma Coater
For coating of conductive thin films
on scanning electron microscopy
samples

Filgen, Inc.

OverviewNo charging. No grains. No heat damages.
An ultimate solution to obtain clear SEM images.

Osmium Plasma Coater
The Osmium Plasma Coater is a kind of plasma CVD coater which is utilizing a method for coating samples in thenegative glow phase domain of DC plasma discharging. As conventional types of metal coaters, there are various kindsof so called sputter coater which use the heavy metals as coating material, such as gold, platinum, palladium etc.
With these methods, the problem of granularity of coating itself is inevitable by any means. Also, if examined at highmagnification, the specimens coated by these methods can not avoid charging, heat damage and contamination causedby exposure to strong electron beam with SEM, resulting in lower resolution of SEM image.
A gas reactor in which the anode and cathode plates are placed verticallyis evacuated to a high vacuum, then sublimated osmium tetroxide (OsO4)
is introduced, and a DC glow discharge is generated under certain
conditions, while maintaining a predetermined gas pressure. The osmium
metal molecules excited by the collision of electrons instantaneously
become plasma between the two electrodes. In particular, in the negative
glow phase domain, there is strong light emission due to the fierce
diffusion of the concentrated positively ionized metal molecules. As aresult, on the surface of the specimen placed in this negative glow phase,the positive ion metal molecules uniformly adhere to the specimen
surface and form a perfectly amorphous metal coating of molecular level,
which molds the microstructure of the specimen surface faithfully.

Applications
Osmium thin film•••••

Conductive thin film for SEM specimen
Prevention of contamination for SEM/TEM specimen
Protective film for AFM specimen
Conductive protective film for SPM specimen
Protective film for SPM cantilever

Osmium ultra-thin film [optional]• Observation of the ultrafine structure of insulators by FESEM• Quantitative analysis of top surface of insulators byESCA/AES• Enhancement of conductivity for TEM specimen• Static prevention treatment for AFM specimen• Antistatic treatment for STM specimen• Etching (Mixed gas method only)

Plasma-polymerized film (naphthalene)
••
•
•
•

Protective film for FIB specimen
Prevention for peeling sample from embedding resin
Coating for fluorine resin (Os-PF hybrid coating)Support film for TEM grid
Drift prevention for ultra-thin sections for TEM

Hydrophilizing treatment [optional]• Pre-hydrophilization treatment for osmium coating on
fluoro resin surface etc.
• Prevention for peeling sample from embedding resin• Hydrophilization of the support film surface for TEM• Hydrophilization of grids for TEM• Hydrophilization of a diamond knife for ultramicrotome• Improvement of wettability

Deep well electrode [optional]• Coating for samples with a height➊Multiple safety measures provide operator
protection from OsO4 exposure.

Benefits
Osmium film

Plasma-polymerized film (naphthalene)

No grains: amorphous metal coating is formed
No heat damage: coating is proceed under room temp.
No electron beam damage: the melting temperature ofOsmium is 2700 deg C
No contamination: coating is started from vacuum state

Strong film: withstand the gallium ions beams used in FIB
Heat resistant and insulated film
No grains: amorphous metal coating is formed
No heat damage: coating is proceed under room temp.
No electron beam damage
No contamination: coating is started from vacuum state

Usability

SafetyAutomatic: whole process is completed just by pressing
START button after settings
Intuitive: coating thickness is controlled by thickness setting,not by discharge time
Short coating time: a few nm/a few seconds
Easy to exchange Os ampoule: detachable reservoir,
observation window (for checking of remaining amount ofOs) and built-in ampoule cutter on reservoirFully automated: reduce chance of human error
Safety features on Os reservoir: gas port integrated
locking pin and built-ion ampoule cutterInterlocking system with reaction chamber: unable toopen the chamber unless OsO4 is exhausted, unable tointroduce OsO4 when the chamber open
Failsafe to prevent Os leak at power down
Osmium absorption filter: not require any ventilator

Safety features on osmium reservoir
Filgen’s OsO4 reservoir is equipped with some safety measures including a mechanical interlocking system forsafety operation.
• Gas-tight and robust design• Safety interlocking system with gas port integrated locking pin (see below)• Built-in ampoule cutter: can reduce risks for exposure to toxic OsO4 gas.
• Observation window: can check remaining amount of OsO4 crystals• Detachable from main unit and can be stored in freezer
The gas port integrated locking pin of reservoir can simultaneously control status for reservoir locking and gas
supply in safe.

Full-opened (during operation)
Reservoir： locked (undetachable) by
manually inserted locking pin ofreservoir
OsO4 gas： can be introduced(depends on solenoid status)

Half-closed (before reservoirdetach)
Reservoir： locked (undetachable) by
manually inserted locking pin ofreservoir
OsO4 gas： blocked *residual gas in
the inlet pipe must be evacuated at
this step

Full-closed (after operation)
Reservoir： unlocked (detachable)
OsO4 gas： blocked➋

Product line-up

Optional units
Conductive ultra-thin film coating system
Osmium film dedicatedmodel #OPC60A

Coating type: Osmium
Thickness: 0.5 to 3.0 nanometer

Low-current method
Forming a film with very low discharge current by graduallyintroducing OsO4 gas to highly vacuumed chamber with applying
voltage. This enables to enhance reproducibility of coating
thickness by lowering uncontrollable over current generated at initial
phase of plasma discharge

Coating type: Osmium
Thickness: several nanometer tohundreds nanometer

Osmium / Plasmapolymerized film model#OPC80T+

Mixed-gas method
Forming a film slowly with relatively low concentration of OsO4 gas
by mixing an inactive gas to chamber. By discharging only with airor other inactive gas, it is also possible to etch your sample.

Hydrophilizing treatment system
Enhance adhesiveness of coating to
your samples by applying this feature
before coating

Deep well electrode
Enable to coat your samples that havea height up to 44 mm.

Coating type: Osmium / PF (napthalene)
Thickness: several nanometer tohundreds nanometer

Accessories➌

Osmium reservoir

Transportation Container

Detachable, equipped with safety features.

Enable safer transportation for OsO4reservoir. Stainless steel made.

OsO4 ampoules

With exclusive optional units, Filgen's OPC
provide a variety of pretreatment methods
for your EM samples

Specifications – base unitsTypeModel #Reaction chamberMax. sample size
Supported SEM
specimen mounts
Coating thickness
Settable min.
thickness

Osmium / Plasma-polymerized film model
OPC80T
Glass chamber, 160(φ) x 105(H) mm44(W) x 44(D) x 4(H) mm or 32(φ) x 14(H) mm

Osmium film dedicated model
OPC60A
Glass chamber, 120(φ) x 73(H) mm33(W) x 33(D) x 4(H) mm or 36(φ) x 14(H) mm

10 mmφ x 2 pcs and 15 mmφ x 2 pcs and 32 mmφ x 1 pc.

10 mmφ x 7 pcs or 15 mmφ x 4 pcs or 36 mmφ x 1 pc.

Coating type
OsO4 reservoir
features
Naphthalene
reservoir featuresGas
introduce/exhaust
methodPower requirements
Dimensions
WeightSeveral nanometers to hundreds of nanometers
Ultra-thin film mode: 0.1 nm / Normal mode: 1 nm
Osmium conductive film, Plasma-polymerized film
Osmium film
(napthalene)
Detachable (capable to store in freezer) / Gas port integrated safety locking pin / Observation window /Built-in ampoule cutter
Heater for effective sublimation / Observation
window
Automated control with vacuum gauge, solenoids, and vacuum pump
100VAC (single-phase) 50/60Hz 12A (including supply
to a vacuum pump)450(w) x 410(D) x 390(H) mm
Approx. 30kg

100VAC (single-phase) 50/60Hz 10A (including supply
to a vacuum pump)450(w) x 390(D) x 340(H) mm
Approx. 20kg

Vacuum rotary pump (supplied with Osmium absorption filter)
Power requirements
Full-load current
Actual pumping
speed
Dimensions
Weight100VAC (single-phase) 50Hz(60Hz) 550W
9.0A (8.4A)

100VAC (single-phase) 50Hz(60Hz) 200W
5.6A (4.8A)

200L(240L) /min

50L(60L) /min

170(W) x 520(L) x 560(H) mm
Approx. 31kg

170(W) x 400(L) x 580(H) mm
Approx. 18kg

Specifications – optional units
Conductive ultra-thin film coating system (low-current method)
Coating typeCoating thickness
Gas introduce method

Osmium conductive ultra-thin film
0.5〜3.0 nm
Needle valve

Conductive ultra-thin film coating system (mixed-gas method)
Coating typeGas introduce method
Supported gas
Dimensions

Osmium conductive ultra-thin film
Mass-flow controller
N2、Ar、He、O2570(w)×410(D)×390(H)mm*This option cannot be installed along with hydrophilizing treatment system

Hydrophilizing treatment system
Gas introduce method
Supported gas
Dimensions

Needle valveAir570(w) x 410(D) x 390(H) mm570(w) x 390(D) x 340(H) mm*This option cannot be installed along with Conductive ultra-thin film coating system (mixed-gas method)

Deep well electrode
Reaction chamber
Glass chamber, 160(φ) x 125(H) mm
Glass chamber, 120(φ) x 103(H) mm
Max. sample size
44(W) x 44(D) x 4(H)mm or 46(φ) x 44(H) mm
33(W) x 33(D) x 4(H) mm or 36(φ) x 44(H) mm
Supported SEM
10 mmφ x 16 pcs or 15 mmφ x 7 pcs or 46 mmφ x 1 pc.10 mmφ x 7 pcs or 15 mmφ x 4 pcs or 36 mmφ x 1 pc.
specimen mounts
Dimensions
450(w) x 410(D) x 410(H) mm450(w) x 390(D) x 370(H) mm➍Technical data

Comparison data: Osmium plasma coat vs. Sputter coat
Sample: Human Lymphocyte

Filgen’s OPC

Ion beam sputter coater

Coating Device: OPC
Coating Material: Osmium
Coating Thickness: 5 nm
Accelerating Voltage: 15.0 kV

Direct Magnification: 10,000X

Coating Device: Ion Beam Sputter
Coating Material: Pt-Pd
Coating Thickness: 8 nm
Accelerating Voltage: 15.0 kV

Direct Magnification: 10,000X

Grains of Pt-Pd are observed at higher magnification

Highly smooth coating surface

Direct Magnification: 50,000X

Direct Magnification: 50,000X

Sample: Barium Titanate

Filgen’s OPC

Direct Magnification: 10,000X

Direct Magnification: 100,000X

Coating Device: Osmium Plasma Coater
Coating Material: Osmium
Coating Thickness: 3 nm
Accelerating Voltage: 10.0 kV➎

Magnetron sputter coater

Direct Magnification: 10,000X

Ion beam sputter coater

Direct Magnification: 10,000X

Horizontal bright and darkbands are observed due tocharging

Horizontal bright and darkbands are observed due tocharging

Direct Magnification: 100,000X

Direct Magnification: 100,000X

Coating Device: Magnetron Sputter
Coating Material: Pt-Pd
Coating Thickness: 3 nm
Accelerating Voltage: 10.0 kV

Coating Device: Ion Beam Sputter
Coating Material: W
Coating Thickness: 1.5 nm
Accelerating Voltage: 10.0 kVHybrid coating with osmium film and plasma-polymerized film
By coating with plasma-polymerized film of naphthalene before osmium coating, a hybrid film which enables toprotect samples, reduce peeling of resin block, as well as prevent surface charging is obtained. This hybrid film issuitable to prepare SEM samples of non-conductive hydrophobic material like fluororesin.

Comparison data: Osmium single coat vs. hybrid coat
Sample: fluororesin film, 0.3 mm thickness

Osmium single coat
Osmium coat: 5 nm

Hybrid coat
PN coat: 2 nm
+Osmium coat: 3 nm

Evaluation for repeatability
Sample: epoxy block
Experimental protocol
1.

2.
3.

Thickness

Coat osmium and naphthalene alternately on an epoxy block,
Naphthalene film: 10 nm, 6 layers
Osmium film: 1.0 nm, 5 layers
Re-embed the sample by epoxy resin,
Prepare cross sections with ultra microtome, then observe with TEM.

For more details, please check our website: https://filgen.jp/Product/SI/English/OPC/technical.html➏Filgen, Inc.
Scientific Instruments Dept.
1-1409 Jonoyama, Midori-ku, Nagoya 459-8011
JAPANTEL: +81 52-624-4388
Email: si-support@filgen.jp
https://filgen.jp/(OCT 2019)