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Description 1, title of the invention
Method of manufacturing boron coating
3. Detailed Description of the Invention The present invention relates to a method of chemically
depositing boron on a substrate under reduced pressure conditions. Methods for chemically
attaching boron onto a substrate, in particular onto filaments, are described in UK Patent No.
1051 3 and 1177854 and Japanese Patent Publication Nos. 49-4137 and 48-27180. The lines of
tungsten, molybdenum, etc. are passed through the mercury sealed reaction tube as it is, and
these lines are mixed with hydrogen in a state where the lines are directly energized (the line
temperature is made 1 oO o o C to 14 o o C). The boron trichloride and the reaction gas
consisting of boron tribromide were flowed to deposit boron on the line. However, the boron
coating obtained by the method described above has the following disadvantages. That is, since
the mercury adheres to the tungsten wire which has passed through the mercury seal, the
mercury reacts with the boron to form a solid mercury halide. Therefore, it is difficult to obtain a
high elastic modulus boron film. Further, in the above-mentioned UK and Japan patents, since the
decomposition deposition reaction of boron is precipitated at normal pressure and at a high
temperature of 1000 ° C. or more, it is difficult to form a dense, uniform EndPage: 1 borondestructed film. . In addition, it reacts with the substrate to form a boron and a hybrid compound
layer of the substrate (for example, a polide layer) over the space between the substrate and the
deposited boron layer. For these reasons, it is difficult to obtain a high elastic modulus boron
coating necessary for an acoustic component. Further, for example, when producing a boron pipe
or plate by chemical work, or the like, there is a disadvantage that a porous pipe or plate can be
produced if the amount of this pride layer is large. The object of the present invention is to
eliminate the drawbacks of the above-mentioned conventional methods and to obtain a boron
coating having a high elastic modulus. That is, the present invention is characterized in that the
boron coating is deposited by controlling the mixing ratio of the gas flow meter and the gas in
the reduced pressure crucible, and an embodiment of the present invention will be described
below. The figure is a schematic block diagram of a low pressure chemical vapor deposition
apparatus. 1 is a bomb of boron halide, 2 is a bomb of hydrogen, 3 is a vacuum gauge, 4 is a
reaction tube, 5 is a wire of sample, 6 is a device for heating sample 6, 7 is an exhaust gas trap, 8
is a vacuum pump is there. (An example in which such a coating is used to deposit a boron
coating on a substrate will now be described. First, a titanium wire is attached to the sample
holder 6 in the reaction tube 4 (for example, a quartz tube or the like). Next, the vacuum pump 8
is operated to obtain the desired degree of vacuum.
After that, the residue is flowed from the cylinder 1.2 of borogen borogen and hydrogen, the
power of the heating device 6 is turned on, the titanium wire is heated, and boron is deposited on
the titanium wire by reductive decomposition reaction as shown in the following formula. 2BXs +
3H2 → 2B + 6HXs (where X is a C1l, Br, I, etc. · · logogen element) Next, the titanium wire is
removed by a chemical process, a etching method or the like to make a pipe-shaped boron rod. If
boron is deposited on the plate instead of the wire and then the titanium plate is removed by
chemical bending balls or the like, the boron plate can be changed. Next, the elastic modulus E of
these pipes and plates is measured. It is needless to say that a material having excellent vibration
characteristics as an acoustic component needs a thick one having an elastic modulus (EKg /
mA). More specifically, a titanium wire of about 100 M in diameter of 30 / lm is attached to a
holding table in a quartz tube having a diameter of 60 and a normal length of 90011 a. . Next,
while drawing air in the quartz tube with a vacuum pump, boron pentachloride is flowed at 5 od
/ min and hydrogen is flowed at 1000 IIIe / min (ratio of boron trichloride to hydrogen 1/20).
Then adjust the pressure to 20 Torr. The temperature of the titanium wire was then raised to
900 ° C. by a heater attached to the outside of the quartz tube, and the reaction was continued
until boron was deposited to 300 μm. Subsequently, titanium which is a core was dissolved and
removed to prepare a pipe-like boron rod. The modulus of elasticity (E) of this bite was 4310
μm. The results are shown in sample No. 1 in the following table. Boron covered IIK was
deposited on the titanium wire in the same manner as in the following two examples. The flow
ratio pressure heating temperature specific elastic modulus of the flows FH2 and BCd3 of boron
hydride and hydrogen at that time is shown in the sample numbers (2) to (16) in the following
table. However, sample numbers (12) to (16) are comparative examples. In the present invention,
a titanium wire was used as the core wire, but in the case of wires such as Aa, Mo, Cu, C1W, Ni,
Ta, Pt, etc., the same experimental results were obtained. Also with Norogen Boron. Then, boron
trichloride (BCav'yk was used, but almost the same experimental results were obtained with r3 °
BI3 for B. The sample numbers (1) to (4) are data when the flow ratio of BCe3 and H2 is changed
with the pressure (20 Torr) and the heating temperature v (900 ° C.) fixed. The sample numbers
(5) to (8) are the values when the flow rate ratio (20 to 1) of H2 to BCe 5 and the heating
temperature (goo'c) are constant and the pressure is changed. Sample numbers (9) to (11) are
data when the heating temperature is changed with the flow ratio of H2 to Bα6 and the pressure
being constant.
Sample numbers (12) to (16) are comparative examples. The pressure of the reaction tube is 200.1 Torr and the heating temperature is 80 ° C. to 9 oo ° as shown in the examples (sample
numbers (1) to (11)) and the comparative examples (12) to (16) in the following table. It can be
seen that, when C, a flow ratio of H2 to BCRs of 20: 1 to 1:10 can provide a boron ruptured film
having a large specific elastic modulus. Also, if the pressure is 20 Torr or more, deposition of the
boron fractured film is too early to form a dense film because the pressure is too low; if it is less
than ITorr, the pressure is too low to obtain a good film, it is difficult to be obtained, and the
heating temperature is 900 ° C. or more In this case, the reaction occurs with EndPage: 2 core
wire to lower the specific elastic modulus, and at 800 ° C. or less, the adhesion of boron is weak
and a good film can not be obtained. It is also understood that when the flow ratio of H2 to BClv
is more than 20: 1, the deposition rate of the boron film is slow and less than 1: 1, so that a good
film can not be obtained. According to the present invention, a boron film having a high elastic
modulus can be obtained by precipitating boron according to the present invention under
reduced pressure conditions such as 1 ', 7'2 to 16 fdJ and 7' tiU.
4, a simplified illustration of the drawing is a principle view of an apparatus for carrying out the
method of manufacturing a boron film of the present invention. 1) Boron trichloride cylinder, 2 ...
hydrogen cylinder, 3 pressure meter, 4 reaction tube, 5 sample holder, θ heating device, exhaust
gas gas tiger . Name of agent Attorney Nakao To one other person 4S2 procedure correction
book Akirari 1! 2 years 72 swords / de 11 patent application No. 101,313 J 2 Title of the
invention 2 Title of the invention Method of manufacturing boron coating 3 Relationship with
person making correction Patent applicant address Osaka Prefecture Kadoma city Ogata Kadoma
1006 Name (582) Representative Matsushita Electric Industrial Co., Ltd. Representative
Toshihiko Yamashita 4 Agent 〒 517 Address Dog Sales Office Kadoma City Oji Kad 真 100
Address Matsushita Electric Industrial Co., Ltd. EndPage: 3, 6, Contents of correction (1)
Description 5th page We will correct 431o% / JJ on the 11th line as 43100KIP / − .
(The table on page 7 of the book will be corrected as follows. 「EndPage: 4