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Technical article

January 2015

42

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this results in a very rough surface, given

the very high surface energy of diamond.

Since diamond is the hardest material

known, the polishing methods are difficult

to apply and very time consuming,

especially for thin diamond films.

The friction coefficient increases as

diamond films grow rougher. Such surface

roughness is not appropriate for many

applications, especially in aluminium

conductor drawing applications which

benefit greatly from the very low friction

of process and very high finish of product,

both of which are now provided by HFCVD

films.

2 Preparation of

nanocrystalline

diamond composite

coating dies

(nano-dies)

The authors of this paper solved the

problem of high surface roughness

of multi-crystalline diamond coatings

by the deposition of nanocrystalline

diamond composite coatings. Composite

diamond films with a smooth surface

were deposited by a two-step chemical

vapour deposition procedure, including

first the deposition of the conventional

rough multi-crystalline diamond and then

nanocrystalline diamond layers.

Cemented tungsten carbide YG6 (Co

6%) drawing dies were used as the

substrates, which were pre-treated by

various methods including leaching

cobalt by dipping in specific reagents

and by scratching the substrate using

diamond powders

[3]

. Conventional and

nanocrystalline diamond films were

deposited in a bias-enhanced hot filament

CVD apparatus.

Nanocrystalline

diamond

thin

films

were continuously deposited in situ

on 10~15μm thickness conventional

diamond films by adjusting CVD process

parameters (such as gas pressure,

hydrocarbon-hydrogen gas mixture ratio

and whether or not bias voltage is applied)

to significantly enhance the secondary

nucleation.

Composite diamond films with a smooth

surface were achieved by the deposition of

alternate rough multi-crystalline diamond

and smooth fine-grained nanocrystalline

diamond layers

[4]

.

A single straight tantalum filament was

arranged to lie on the centre line of the die

to be coated (see

Figure 1

).

The tantalum wire is held straight by

a high temperature spring or a kind of

specially designed holder in the case of

very small bore diameter dies. A single

straight filament located at the axis

centre of the die can maintain uniform

temperature on the surface of the bore

of the drawing die during the deposition

process.

A DC bias is applied between the filament

and the drawing die substrate so as to

enhance the diamond nucleation density.

3 Characterisation

and discussion of

nanocrystalline

diamond composite

coating dies

(nano-dies)

Figures 2a

and

2b

show the surface

morphology

of

conventional

multi-

crystalline and nanocrystalline diamond

coatings. For conventional multi-crystalline

diamond, as shown in

Figure 2a

, the film

displays a well-faceted microcrystalline

diamond surface with grain size ranging

from 2 to 4μm.

The surface is very rough and consists of

a combination of {111} and {110} facets.

For nanocrystalline diamond, as shown

in

Figure 2b

, the film appears very dense

with a fine-grained morphology (grain

size about 50nm). The surface morphology

is non-faceted and much smoother than

multi-crystalline diamond films.

Figure 3

shows the Raman spectrum of the

composite coatings of multi-crystalline

diamond

film

and

nanocrystalline

diamond

film.

For

conventional

multi-crystalline diamond films, the only

sharp characteristic peak for diamond (sp

3

carbon) appears at 1,332cm

-1

.

For nanocrystalline diamond films, a

characteristic peak for diamond (sp

3

carbon) appears near 1,339cm

-1

. And a

broad peak near 1,580cm

-1

corresponds

to amorphous carbon or non-diamond

carbon (sp

2

carbon). It can be inferred

that the conventional multi-crystalline

diamond film contains much less

non-diamond component.

For

nanocrystalline

diamond,

the

diamond band at 1,332cm

-1

is significantly

Figure 2

:

The plane-view SEM images of the multi-crystalline and nanocrystalline diamond coating

(a)

(b)

Figure 4

:

Appearance of nanocrystalline diamond

composite coatings die (nano-die)

Figure 3

:

Raman spectra of the multi-crystalline

coating (black) and nanocrystalline diamond

coating (red)

intensity (au)

wavenumber (cm

-1

)

underlying MCD film

surface NCD film