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Description 1, title of the invention
Boron structural material and method for manufacturing the same
3. Detailed Description of the Invention The present invention relates to a method for producing
a boron structural material, and in particular to improve the film quality and mechanical
properties of boron constituting the boron structural material. Boron is a useful material for
cutting tools, sliding machine parts, bearings, etc. because it has the second highest hardness
after diamond and its wear resistance is also very high. Also, the specific elastic modulus (elastic
modulus / density) Among the substances currently known, it has the excellent feature of
maximum. This 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 boronapplied products in a dense mass by methods such as casting and rolling, and therefore, in the
production of various boron-applied products, in most cases, materials other than boron are
used. The substrate is used as a composite having a boron coating formed by vapor deposition,
sputtering wave, chemical vapor deposition (CVD) or the like. In such a conventional method (Ha,
the hardness of boron and its EndPage: 1 In the case of products utilizing excellent abrasion
resistance, there is no major hindrance. However, the use of the size of the specific elastic
modulus, the diaphragm of the speaker, the force of the cartridge, the acoustic material such as
the lever or the like, and the sword become extremely serious obstacles. That is, the density and
elastic modulus of the bonded body largely depend on the properties of the substrate, and the
intrinsic properties of boron are thereby largely reduced. On the other hand, conventional boron
coatings were amorphous ones alone, crystalline ones alone, or mixed crystals of these materials,
but such amorphous single ones, crystalline (β- In the case of rhombedral, alpha-rhombedral
tetragonal, etc.) alone, boron with sufficient mechanical strength can be obtained due to the
influence of thermal strain during CVD, and distortion and cracks that enter the boron when
dissolving and removing the substrate metal. Was difficult. On the other hand, amorphous and
crystalline mixed crystals are also inhomogeneous in the boron body and are affected by the
thermal strain that occurs during CVD, and a film having sufficient mechanical strength is not
obtained. We have used tantalum (Ta), niobium (Nb), molybdenum (h-o), tungsten (W), titanium
(1 °) coated with borides of chromium or Or to eliminate such conventional drawbacks. i) on a
metal substrate such as Chemical Vapor Deposition (CVD) L of crystalline boron, then CVD of
amorphous boron on top of this, then a double layer boron coating obtained by dissolving away
the metal substrate? , It was found to have excellent mechanical strength.
1 and 2 are one example of a pipe-like and flat-like one, in which 1 is a crystalline layer and 2 is
an amorphous 9 layer. The method of forming boron on a substrate by a chemical vapor
deposition method (CVD method) is, for example, heating the substrate placed in a reactor by
infrared heating, high frequency heating, energization, etc. and reducing decomposition reaction
as shown in the following formula Precipitate semen. 2BX '+ 3H2.fwdarw.2B + 6HX (where X is
C.sub.4 Br, I,........... Rogen elements) As source gases used for the CVD method, there are hydrides
of boron and the like in addition to BX3. In addition, in this boron precipitation reaction, the
crystal form of the gods is obtained by the heating temperature, the gas pressure, the inflow of
the raw material gas to the reactor, and the like. Next, the substrate is dissolved and removed by
a chemical method to obtain a pipe plate mainly composed of boron alone. As a liquid having
such a chemical action, a liquid mainly containing hydrofluoric acid can be considered. Further,
as a particularly effective solution, there is a solution obtained by dissolving bromine, chlorine,
iodine, or two or more of these compounds (iodine trichloride, -iodine chloride etc.) or a mixture
in anhydrous alcohol-as a metal substrate Tantalum, niobium, molybdenum, tungsten, titanium
and the like are preferable because CVD of boron is carried out at a high temperature (900 ° C.
or higher) and it is easy to heat the substrate by energization. In addition, tantalum and
molybdenum have a low degree of hydrogen layering because CVD is performed in a hydrogen
stream. Tungsten is more desirable. In addition, it occurs in the process of dissolving and
removing the above metal substrate by coating chromium or a boride of chromium on these gold
substrates by electroplating, CVD, vacuum evaporation, sputtering or the like. The strain can be
removed and the strength of the boron coating is increased. As mentioned above, crystalline
boron is chemically vapor deposited on a Cr coated metal substrate, then amorphous silicon is
chemically vapor deposited for this crystal inhibition, and then Cr coated metal substrate The
double-layer boron obtained by dissolving and removing has significantly improved mechanical
strength as compared to the conventional boron single layer or the mixed layer boron f. Further
details will be described in the examples. EXAMPLE A tantalum wire having a diameter of 250
microns and a length of 800 M was prepared. After degreasing and washing, the coated tantalum
wire is heated to 1250 'C by applying a current to 0 for about 1 micron of chromium coated by
I10 sputtering, and 1 part by volume of boron trichloride (BσU) and hydrogen (82 Three parts
by volume were flushed at a rate of 1β / min for 1 minute-(at this time boron deposited to a
thickness of about 25 microns).
As a result of X-ray diffraction, the crystal form of the element p1 was β-longohedral. Next, this
line was energized and EndPage: 2 heated to 900 'C, and the same <BC β 51 parts by volume
was used, and z3 parts by volume was flowed at a rate of 1 β / min for 2 minutes. (At this time,
it was confirmed by X-ray diffraction that about 25 μm of amorphous boron was attached to the
β-rombohedral 碍, element. The sample thus prepared was cut into 5 gates and immersed in a
commercially available anhydrous methanol 200 m 71 in which bromine sogr was made to have
an angle of 4 to dissolve tantalum and coated chromium. (The boron does not dissolve at this
time. 2.) A pipe consisting of a double layer of platinum and rhombohetrales 1 and amorphous
boron (, 1, inner diameter 260 μm, outer diameter 350 μm, length 5 M 1) Measure the bending
strength of this pipe did. The length of the beam is set to 4 M, and the load W is applied in the
form of both-end support beams, and the average strength of the samples (20 pieces) cut into
51′J is obtained as a result of the load. The breaking strength was 710 gr. The results are
shown in the sample layer (1) of Table 1. A boron structural material was obtained in the same
manner as in the following examples. The results are shown in Table 1 However, although the
sample numbers (° 0) to ("2") correspond to 1 Comparative example 1 · 6 · sample layer-E-ヱ 粂,
the inner diameter and outer diameter of the boron structural material are respectively 250
"μm, 350) The time of CVD was controlled so as to be constant at tan (thickness: 50 '\, constant
at 7 · μln). In the first one and the table, 250 μm tantalum wire was used as the metal substrate,
but the same may be applied to the shape of the gold plating substrate and the type of substrate
(others in which Mo, Nb, Ti and V were tried). The results were obtained. Also, if the crystalline
layer and the amorphous layer are separately divided into n layers, that is, multiple layers of
CVD1 each having 17 and 17 layers respectively (however, base or crystal 7tIi4 = on top of that)
There is no formation of an amorphous layer. 2.) Crystalline layer, 2K after amorphous t '↓, "H",
and it turned out that the same result was obtained from one end to the other. As is apparent
from the examples [sample numbers (1) to (9)] of the table and the comparative examples
[sample numbers (10) to (12)], an amorphous 1 layer (non It can be seen that the double-layered
boron structural material to which the crystalline layer is attached has a high mechanical
strength and a high mechanical strength, and its industrial value is great.
j, 4 Brief Description of the Drawings FIGS. 1 and 2 are cutaway views showing boron structural
materials in an embodiment of the present invention. 1 · · · crystalline layer, 2 · · · amorphous
layer. Name of agent Attorney Nakao Toshio or one EndPage: 3
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