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Description 1, title of the invention
Method of manufacturing boron structural material
3. Detailed Description of the Invention The present invention relates to a method for producing
a boron structural material, and in particular, the improvement of the film quality and
mechanical properties of boron constituting the boron structural material, and the production,
retention and productivity of the boron structural material. The purpose is to work as above.
111, boron has the second highest hardness after tire monde, and has the best characteristics
among the materials. This property means that the propagation velocity of the sound wave is the
largest in the existing materials, and is particularly useful as an acoustic material. It is difficult to
obtain boron-applied products in the form of dense lumps, thin plates, thin-walled pipes, etc. by
casting or rolling. Therefore, in the manufacture of various boron applied products, in most
cases, boron is deposited on a substrate made of a material other than boron by a vapor
deposition method, a sputtering method, a chemical vapor deposition method (hereinafter
referred to as a CVD method). It is used as a complex in which a boron film is formed on a
substrate made of other materials. Composite structural materials made by such conventional
methods do not cause significant problems in the case of products that utilize the hardness of
boron and its excellent wear resistance. However, in the case of the acoustic material of the
speaker diaphragm or the cartridge EndPage: 1 each lever which intends to utilize the size of the
specific elastic modulus, it becomes a serious trouble. That is, the density and elastic modulus of
the composite largely depend on the nature of the substrate, and the intrinsic nature of boron is
thereby largely reduced. On the other hand, there have been many attempts to separate boron
from the substrate by chemical or physical treatment, but distortion occurs due to the difference
in thermal expansion coefficient between the deposited boron film and the substrate, which
causes the boron film to It was difficult to obtain a boron film having sufficient mechanical
strength with good yield due to cracking and the like. In order to eliminate the drawbacks
present in such conventional methods, the present inventors are based on metals such as
tantalum, niobium, molybdenum, tungsten, titanium and the like, and 6.5 mol% to 65.0 vanadium
on the surface thereof. It has been found that depositing chromium containing mole% to a
desired thickness and chemical vapor deposition on this is effective. Hereinafter, the method of
the present invention will be specifically described. In order to form boron on a substrate by a
CVD method, for example, a substrate placed in a reactor is heated by infrared light or 1112 B О
3 3 H 2 ? 2 B + 6 H X (where X is a halogen element such as C 1, Br, I). In addition to boron
halide BX3, as a raw material gas used for the CVD method, there are also hydrogen compounds
of boron and the like.
In addition, in this boron precipitation reaction, 1 various crystal forms can be obtained by
heating and heating, and raw materials to the reactor by this inflow type and the like. Of the
various crystal forms. In order to have a compact, excellent mechanical property and a d-boron
film, it is desirable to use ?-rhombedral, tetragonal or amorphous iodine. Next, the substrate is
dissolved and removed or peeled off by a chemical or mechanical method to obtain a pipe or
plate made of boron alone in the king. As the chemical method, it is considered to use a solution
mainly made of hydrofluoric acid. ????? Further, as particularly effective liquids, there are
those in which bromine, chlorine, iodine, and two or more of these compounds or mixtures are
dissolved in anhydrous alcohol as a liquid. As the base metal, tantalum, niobium, morpden,
tantalum, niobium, morpden, and the like are considered because the CVD of boron is performed
at high temperature (900 ░ C. or higher) and it is easy to apply current and high frequency
heating. Titanium, tungsten, etc. are desirable. Among these materials, tantalum, molybdenum
and tungsten, which have a low degree of hydrogen embrittlement, are more desirable because
CVD is carried out in a hydrogen stream. In order to reduce the thermal strain between the
precipitated boron film and the substrate, tantalum or titanium having a thermal expansion
coefficient close to boron is more preferable. The main point of the method of the present
invention is that chromium containing not more than 5.5 mol tl) to 65.0 moles of chromium is
deposited on the above metal by an electric plating method, a CVD method, a sputtering method,
a vacuum evaporation method, etc. , It is to be bombarded with a layer of a desired thickness to
form a substrate. Thereafter, it is deposited on a boron f substrate, and then the substrate is
selectively dissolved and / or mechanically removed to form a structure consisting of a snail. You
get things. Conventionally, when using only a metal substrate or a substrate from which only
chromium is extracted on the metal substrate. In the process of selective melting and mechanical
peeling, the boron film may be broken or the mechanical properties of the obtained boron
structure may not be very good. The method of the present invention provides an improvement
in these respects. In particular, when the boron was amorphous, it was greatly improved. Thus,
for example, when the substrate is linear, a pipe-like boron structural material is obtained, and
when it is plate-like, a thin plate-like ovarian structural material is obtained. The yield of the pipe
obtained by leaving is not very good. Also, if it is more than 65 moles, the substrate is deformed
during boron CVD, and the strength of the boron is reduced. When a chromium-containing plate
containing vanadium is used as the it substrate, the substrate itself generates an EndPage: 2
shape when the temperature is high at the time of CVD, so the boron film is cracked at the end of
the CVD of boron .
Therefore, in order to exert the effects of the present invention, the thickness of the chromium
layer containing 5.6 moles of vanadium to -65, O moles 6 has a desirable thickness. The desired
thickness also depends on the thickness of the substrate metal. When linear tantalum having a
thickness of, for example, 200 to 300 ?m was used as the base metal, the thickness of the
vanadium-containing chromium layer was 10 ?m or less. If it is too thick, the boron coating
tends to crack. However, if it is about 0.06 ?m, the improvement effect by the present invention
can not be clearly recognized. The thickness of the most favorable coating layer in this case was
0.3 to 2.0 ?m The effect according to the invention is greatest when using tantalum as the metal
of the substrate. It is considered that this is because the thermal expansion coefficient is close to
that of boron and that the degree of hydrogen embrittlement is relatively small. The chromium
layer containing vanadium can be coated on the substrate by electro plating,-) sputtering, or CVD.
Whatever the coating method used, the results were almost the same. Further details will be
described in the examples. A tantalum wire with a diameter of 260 ?m% and a length of 800 m
was prepared. The wire was degreased and cleaned, and then 5.5 mol% of vanadium was
deposited thereon by sputtering gold-chromium to form a layer of about 1.0 ?m. Next, a
tantalum wire coated with a chromium layer containing 5.6 moles of vanadium is heated by
energization to generate heat and hold it at a temperature of 1000 ░ C., and this is irradiated
with boron trichloride (BCl 2) 1 and the like. The solution was dissolved in 200 ml of commercial
anhydrous methanol in which bromine esog was dissolved in 200 ml of commercially available
anhydrous methanol to completely dissolve borides such as tantalum, chromium and vanadium.
At this time, boron does not dissolve. The dimensions of the obtained pipe were an inner
diameter of 250 ?m, an outer diameter of 360 ?m, and a length of 6. As a result of examination
by X-ray diffraction, the crystal form was amorphous to the king (amorphous). The breaking
strength of this pipe was measured. The measurement was carried out in such a manner that load
length W was applied in the form of a support beam with four lengths of beam and one end, and
the load was obtained when the pipe was broken. Next, a sample cut to a gain of 5 from a sample
of length SOO was destroyed by a number of 25% in the process of dissolving and removing the
substrate. That is, the yield was 76 units. The average flexural strength of the obtained pipe
The results are collectively shown as sample 1 in the following table. The samples 2 to 9 shown
in the following table were prepared in the same manner as in the above example, and they were
also examined. 2.) As a method of coating a tantalum wire with chromium containing palladium,
a method of wi-coating by a direct current sputtering method as a powder compact target of
vanadium-chromium was used. The time of CVD was adjusted so that samples 2 to 13 all had a
film thickness of 50 ии ?m. For comparison, boron was deposited to a thickness of 60 ?m each
when coating only with chromium (tantalum wire) (sample 12) or only with tantalum wire
(sample 13). The boron deposition temperature, the yield, the average bending strength, and the
crystal system at that time are also summarized in the following table. According to the following
margin EndPage: 3, the yield of boron pipe is good and the average bending strength is also
large. Particularly for amorphous boron, it is better for the yield strength to contain better than
the chromium coating alone. Although the boron pipe was shown in the said Example, the same
result was obtained with plate-shaped boron. The base is not only tantalum but also
molybdenum, niobium and titanium. Similar results were obtained with tungsten. ???? Add
other elements to chromium besides vanadium. It is also possible to further enhance the effect.
Name of agent Attorney Nakao Toshio and one other EndPage: ?
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