JPH0489199

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DESCRIPTION JPH0489199
[0001]
The present invention relates to a manufacturing method that can be suitably used when forming
a film made of diamond, which is a brittle material, into a diaphragm for a speaker, a corrosionresistant container, etc. A highly brittle material is obtained by stacking the bodies to form a
laminate, then attaching the laminate to a mold having a predetermined shape, and then applying
pressure to deform the laminate in a heated state of 800 to 1500 ° C. It is made to be able to
form a certain diamond film. [Conventional technology] Conventionally, in order to produce a
diamond film shaped body with a thickness of about 40 to 200 μm having a three-dimensional
shape, a substrate to which a desired shape is transferred is made of silicon or the like, The
diamond film was formed by the CVD method or the like, and then the base material was
removed. [Problems to be solved by the invention] When diamond is deposited on the surface of
a substrate having such a complicated shape to produce a diamond film shaped body having a
three-dimensional shape, the thickness of the obtained product is uneven. There was a problem.
In addition, when the shape is complicated, internal stress is unevenly generated when forming a
diamond film, and there is a problem that the diamond film can not withstand deformation at the
time of removing the base material and is easily broken. The present invention has been made in
view of the above circumstances, and it is an object of the present invention to provide a method
for producing a film-like diamond molded body with less variation in film thickness and capable
of avoiding breakage when peeling a diamond film from a substrate. Do. 1 Means for Solving
the Problems In the method of manufacturing a film-like diamond compact according to the
present invention, a plate made of a superplastic material is overlaid on a diamond film. Then, the
laminated plate is attached to a predetermined three-dimensional shape forming die, and then
the laminated plate is deformed by applying pressure to the laminated plate in a state of being
heated to 800 to 1500 ° C. After the laminate is deformed in this manner, a portion of the
superplastic material plate is removed from the laminate to obtain a three-dimensionally shaped
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diamond film. Removal of portions of the superplastic sheet may be after or before removing the
deformed laminate from the mold. It is desirable to apply a mold release agent between the
diamond plate and the superplastic material plate in consideration of the workability of the step
of removing the portion of the superplastic material plate as described above. As a mold release
agent, BN (boron nitride) etc. are suitable. The temperature (hereinafter referred to as processing
temperature) applied when deforming the laminate should be 800-1500 ° C. This temperature
range is mainly determined by the reason of the diamond film side, and the actual processing
temperature is set within the above range and a temperature at which the superplastic material
described later exhibits superplasticity.
If the processing temperature is lower than the above range, the deformation resistance of the
diamond is increased, which causes a disadvantage that a device for generating high pressure is
required. In addition, if the processing temperature exceeds the above range, the graphitization
of diamond may occur. The above-mentioned superplastic material is known as a material which
exhibits several hundreds or more of elongation before fracture when a force is applied under a
certain temperature. Although various superplastic materials are known at present, preferred
ones for use in the present invention are, for example, stainless steel, titanium alloy, Ti-AI alloy,
Ni alloy, norconia, norconia-alumina composite. It is a body etc. Since the temperatures at which
these superplastic materials exhibit superplasticity are different from each other, the processing
temperature at the time of deforming the laminate is appropriately determined depending on the
superplastic material used. The processing temperatures suitable for each of the superplastic
materials are as shown in Table 1. Table 1 A laminate consisting of a superplastic material sheet
and a diamond sheet is a superplastic material sheet laminated on both sides of the diamond
sheet even if the superplastic material sheet is laminated on one side of the diamond sheet It may
be The strain rate at the time of superplastic working here is preferably in the range of 10 to 10
'/ sec. If the speed is higher than this range, the mold may be broken due to the high pressure,
and the uniformity in superplastic deformation may be reduced. In addition, since the
superplastic material plate is exposed to a high temperature for a long time at a slow speed,
crystal grains of the structure of the superplastic material plate may grow and be coarsened, and
the superplasticity may be reduced. Further, it is desirable that the oxygen concentration in the
residue in contact with the diamond plate at the time of superplastic forming is +000 ppm or less
from the viewpoint of preventing the deterioration of the diamond. The molding die used in the
manufacturing method of the present invention may have a molding surface (a ridge on which a
laminate is pressed), a convex shape, or a concave shape. [Operation] According to this method of
manufacturing a film-like diamond compact, a diamond film which is a highly brittle material can
be formed into a desired three-dimensional shape. The inventors of the present invention for this
reason, when forming in a state where a superplastic material plate is laminated on a diamond
film, the diamond plate and the superplastic material plate are simultaneously deformed at the
time of forming, and pressure is evenly applied to each part of the diamond plate. I think that it is
to join. Hereinafter, the method for producing a film-like diamond compact according to the
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present invention will be described in detail with reference to the drawings. (Embodiment 1)
FIGS. 1 to 4 show the steps of an embodiment of the method for producing a film-like diamond
compact according to the present invention.
In this manufacturing method, first, a flat substrate made of silicon was set in a microwave
plasma CVD apparatus, and a diamond film was formed on the substrate surface under the
conditions of a substrate temperature of 800 ° C. and a CH 4 concentration of 0.5 volume%.
Then, as shown in FIG. 1, a release agent (BN) is applied to both the front and back sides of the
obtained 40 μm thick diamond film l, and then a 300 μm thick stainless steel (SUS 329)
superplastic material plate 2.2 was piled up and it was set as the laminated board 3. Next, as
shown in FIG. 2, this laminated plate 3 was attached to a mold 4. The mold 4 is composed of an
upper mold 5 and a lower mold 6, and the laminated plate 3 is held between the upper and lower
molds 5.6 at its peripheral portion. As shown in FIG. 5, the upper mold 5 is formed with a squareshaped recess 7 and a gas injection port 8 is formed in the center thereof. Further, as shown in
FIG. 6, the lower die 6 is formed with a hemispherical concave portion 10. The inner surface of
the concave portion IO is formed in a shape corresponding to the desired shape of the diaphragm
of the speaker. Further, a gas vent It is formed at the center thereof. After setting the laminate 3
in such a mold 4, the laminate 3 is heated to 950 ° C. and f 2. Thereafter, argon gas was blown
into the mold 4 from the gas blowing port 8. Then, as shown in FIG. 3, the laminate 3 was
gradually deformed and finally adhered to the inner surface of the recess IO of the lower die 6.
The gas blowing rate was adjusted so that the strain rate of the laminate 3 was 10 to 37 seconds.
Finally, after holding the gas pressure of 10 kg / mm 2 for 10 minutes, the forming process was
finished. Thereafter, the laminate 3 was taken out of the mold 4 and the superplastic material
plate 2.2 was mechanically removed. As a result, a film-like diamond compact 20 formed as
shown in FIG. 4 was obtained. In this method of manufacturing a film-like diamond compact,
pressure is applied to perform molding while holding the diamond film 1 between the
superplastic alloy plates 2 and 2, so the diamond film l and the superplastic alloy plate 2 are
simultaneously formed during molding. The pressure was applied uniformly to each portion of
the diamond film I so that the diamond film l, which is a highly brittle material, could be formed
into a predetermined diaphragm shape without breakage. And, according to this manufacturing
method, since the diamond film can be formed into a three-dimensional shape, the diamond film
may be formed into a flat shape. In the case of forming a flat diamond film, since the variation in
film thickness is small, according to this manufacturing method, it is possible to manufacture a
three-dimensional shaped diamond compact 20 with less variation in thickness.
Further, according to this manufacturing method, since it is sufficient to form the diamond film 1
in a flat shape having a small internal stress, the problem of breakage of the diamond film l when
removing the formed diamond film l from the substrate is also avoided. it can. (Embodiment 2)
FIGS. 7 and 8 illustrate the second embodiment of the method for producing a film-like diamond
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compact according to the present invention. In the manufacturing method of this embodiment, a
release agent is applied only to the back surface of the diamond film l, and the superplastic alloy
plate 2 is laminated to obtain a laminated plate I3. The laminated plate 13 was set so that the
diamond film l side was positioned on the upper mold 5 side as shown in FIG. 8, and was then
molded by the gas blow method in the same manner as in Example 1. Also in this manufacturing
method, a good film-like diamond compact 20 can be formed as in Example 1. (Embodiment 3)
FIGS. 9 to 12 show steps in a third embodiment of the manufacturing method of the present
invention. In the manufacturing method of this example, first, as shown in FIG. 9, a laminate 3
similar to that of Example 1 was manufactured. Next, this laminate 3 was set in a hot press mold
15 as shown in FIG. This mold consists of the punch 16, the die 17 and the pressing ring 18, and
when the punch 16 and the die 17 are put together, a space having the same shape as the
desired molded body is formed therebetween. There is. The laminate 3 is fixed to the die 17 in a
state where the outer peripheral portion thereof is sandwiched between the upper surface of the
die 17 and the pressing ring 18. After the laminate 3 was thus set in the mold 15, the mold 15
was placed in an argon atmosphere, and then the laminate 3 was heated to 950 ° C. Thereafter,
the punch 16 was lowered gradually. After the punch 16 was lowered to the lowermost portion
as shown in FIG. 11, the punch 16 was raised, and the formed laminate 3 was taken out. When
the portions of the superplastic alloy plates 2 and 2 were mechanically removed from the
laminate 3 thus obtained, the diamond film 1 was formed into a desired shape as shown in FIG.
Also in this manufacturing method, as in the case of Example I, the diamond film 1 could be
formed without being broken. Example 4 A diamond film l was formed under the same conditions
as in Example 1 using the mold 30 shown in FIG. The mold 30 is an upper mold 3 that forms a
rectangular space. And a lower die 32, and a convex die 33 provided in the inside thereof so as to
be vertically movable. In this embodiment, first, the laminated plate 3 is sandwiched between the
upper and lower dies 31.32, and then the convex 33 is moved upward to abut on the laminated
plate 3 as shown in FIG. As shown, argon was blown to the upper mold 31 side to deform the
laminate 3.
Also by the manufacturing method of this embodiment, a good beryllium diaphragm could be
manufactured as in the case of the first embodiment. (Example 5) The beryllium rolled sheet 1
was formed using the lower mold 6 shown in FIG. Also in this method, as in Example 1, a good
beryllium diaphragm could be obtained. [Effects of the Invention] As described above, in the
method for producing a film-like diamond molded body according to the present invention, a
plate made of a superplastic material is stacked on a diamond film to form a laminate, and then
this laminate is given a predetermined three-dimensional shape. The laminate is then heated to a
temperature of 800 to 1500 ° C., and pressure is applied to the laminate to deform it, so that
the diamond film and the superplastic material are deformed simultaneously during molding. The
pressure is evenly applied to each part of the diamond film. Therefore, according to the method
for producing a film-like diamond compact of the present invention, a diamond film which is a
highly brittle material can be shaped into a predetermined three-dimensional shape. And,
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according to this manufacturing method, since a flat diamond film can be formed into a threedimensional shape, the diamond film may be formed into a flat shape. In the case of forming a
flat diamond film, since the variation in film thickness is small, according to this manufacturing
method, a three-dimensional shaped body with less variation in thickness can be manufactured.
Further, in this manufacturing method, since it is sufficient to form the diamond film in a flat
shape having a small internal stress, it is possible to avoid the problem that the diamond film
breaks when removing the formed diamond film from the substrate.
[0002]
Brief description of the drawings
[0003]
1 is a cross-sectional view showing a laminate used in the manufacturing method of Example 1,
FIG. 2 is a cross-sectional view showing the same laminate set in a mold, and FIG. FIG. 4 is a
cross-sectional view showing the film-like diamond compact obtained in Example 1, FIG. 5 is a
bottom view showing the upper mold 5 used in Example 1, and FIG. 6 is Example 1 7 is a crosssectional view showing a laminate used in the manufacturing method of Example 2, and FIG. 8 is
a cross-sectional view showing a state where the laminate is set in a mold. FIG. 9 is a sectional
view showing a laminate used in the manufacturing method of Example 3, FIG. 10 is a sectional
view showing the laminated plate set in a mold, and FIG. 11 is a process of deforming the
laminate FIG. 12 is a cross-sectional view showing the film-like diamond compact obtained in
Example 3, and FIGS. 13 to 15 are manufacturing methods of Example 4. Cross-sectional views
showing process steps, FIG. 16 is a sectional view showing the lower mold used in Example 5.
■ · · Diamond film, 2 · · · Superplastic alloy sheet, · · · · · · · · · · · · · molds, lO · · · recess, 13 · · ·
laminates, 15 · · · hot press mold 20: Film-like diamond compact, 30: mold.
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