JPH10231182A - Fastening member - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a fastening member excellent in heat resistance, slight in reduction in mechanical characteristics with time even in use in an environment of practical use as in the air at room temperature to a high temperature and improved in tensile strength, mechanical strength of screw thread part and environmental resistance. SOLUTION: This fastening material comprises a composite material of an inorganic filament 2 and a glass ceramic 3. The inorganic filament 2 is one or more selected from a silicon carbide based filament, a silicon nitride- based filament and an alumina based filament. The glass ceramic 3 is one comprising Al2 O3 , SiO2 and SrO and/or BaO as essential components.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fastening member used in various fields, and more particularly to an application requiring high heat resistance, high strength, and light weight, for example, useful in the aerospace industry and the like. And fastening members such as bolts and nuts.

[0002]

2. Description of the Related Art For example, in the field of the aerospace industry, fastening members such as bolts and nuts are required to have excellent heat resistance and high specific strength. . For this reason, conventionally, a composite material in which carbon is reinforced with carbon fibers (hereinafter, referred to as a “C / C composite material”)
), Such as bolts and nuts, have been put to practical use. The fastening member made of the above C / C composite material is mainly made by impregnating a carbon fiber 2D fabric with a matrix and firing it to densify it, or cutting out a densified flat plate by CVI or CVD and processing it into a screw or bolt shape. Was obtained by The conventional fastening member thus obtained is apt to break due to shear stress applied between the layers on two surfaces located in a direction perpendicular to the fiber orientation, and the conventional bolt 100 shown in FIG. As described above, it is general to adopt a structure having two surfaces with missing screw threads. For this reason, the fastening member has a disadvantage that the thread is liable to be lost during use because the thread has a cut portion.

In order to make up for this drawback, Japanese Patent Laid-Open Publication No.
No. 1 describes a method for manufacturing a screw member using a carbon fiber reinforced composite material using carbon fiber short fibers as a reinforcing material. However, the thread member obtained by this manufacturing method has a tensile strength of 60 mm when machining M10 threads.
MPa or less, the reinforcing effect of the reinforcing fiber on the tensile stress was low, and the strength was low.

[0004] Japanese Patent Application Laid-Open No. 7-19220 discloses that
A method is described in which prepreg sheets having various fiber orientations are laminated, and a matrix is impregnated, cured or fired to produce a bolt base material. However, in the bolt base material obtained by this manufacturing method, the fiber orientation direction and the direction in which the tensile stress of the bolt is applied are few in number, so that the fiber strength is not sufficiently reflected in the bolt strength, and the tensile strength is also low. , And M10 screws, it was as low as about 100 MPa.

[0005] The C / C composite material has, as a restriction on its production method, a matrix that cannot completely fill the gaps between the fiber bundles and usually has pores of about 5 to 10 vol%. That is, a long fiber reinforced composite material represented by a C / C composite material is generally formed by forming a fiber preform and impregnating the matrix with a gas phase or a liquid phase, or by impregnating a matrix raw material and then converting it. It is obtained by using a matrix. For this reason, pores remain in the matrix of the completed composite material, and it is very difficult to obtain a 100% dense compact. Accordingly, the C / C composite material thus obtained has fine irregularities such as screw threads, and is not suitable as a material for forming a structure on which stress is applied.

[0006] In short, fastening members such as bolts and nuts formed of a C / C composite material are, for example, 2D.
In the case of a flat plate made of a laminated material, although it has a high tensile strength of 300 MPa, when used as a fastening member for a structural material, it can be used only in a field having a considerably low stress, and particularly has a large tightening torque. Can not be used in parts that require. Further, since the C / C composite material is weak against oxidation, it cannot be used at high temperatures unless it is in an inert gas or in a vacuum, and has poor environmental resistance. Was. In order to improve this environmental resistance, SiC / S, which is more stable against oxidation,
Although it is conceivable to use an iC-based composite material, even if such a composite material is used, it usually has pores.
It did not eliminate the same drawbacks as the C / C composite material described above in terms of mechanical strength.

[0007] Accordingly, an object of the present invention is to provide excellent heat resistance,
Furthermore, even when used in the actual use environment such as the atmosphere from room temperature to high temperature, there is little deterioration in mechanical properties over time, and it is excellent in tensile strength, thread part strength and environmental resistance. It is to provide a member.

[0008]

Means for Solving the Problems The present inventors conducted various studies to solve the above-mentioned problems, and as a result, formed a dense composite material using glass ceramics as a matrix and inorganic long fibers as a reinforcing material. It has been found that a fastening member used for a material can achieve the above object.

The present invention has been made based on the above findings, and is made of a composite material of an inorganic long fiber and glass ceramic, wherein the inorganic long fiber is a silicon carbide fiber, a silicon nitride fiber, and an alumina fiber. At least one selected from the group consisting of
there is provided a fastening member, characterized in that l ₂ 0 _3, a glass ceramic containing SiO _2, SrO and / or BaO as an essential component.

[0010] The present invention also provides the fastening member, wherein the glass ceramic further contains MgO.

The present invention also provides the fastening member, wherein the inorganic long fiber is a silicon carbide fiber of the following (1). (1) Substantially Si, Ti and / or Zr, C,
O and an amorphous phase and β of 500 ° or less.
-A crystalline aggregate of SiC and TiC and / or ZrC, or SiOx present in the crystalline and in the vicinity thereof
And an amorphous mixed system composed of TiOx and / or ZrOx (0 <x ≦ 2), and the elemental composition is as follows:
5-60 wt%, Ti and / or Zr 0.2-5 wt%
%, C is 20 to 45 wt%, and O is 0.1 to 20.0 wt%
% Silicon carbide based fiber.

Further, the present invention provides the above-mentioned fastening member, wherein the inorganic long fiber is a silicon carbide fiber of the following (2). (2) The element composition is such that Si is 30 to 80 wt% and C is 20
A silicon carbide fiber having an amorphous content of Si and C and / or a β-SiC crystalline and carbon agglomerate of 10000 ° or less and having an H content of 2% by weight or less and 70% by weight or less.

Further, the present invention provides the above-mentioned fastening member, wherein the inorganic long fiber is a silicon carbide fiber of the following (3). (3) The element composition is such that Si is 30 to 80 wt% and C is 10
~ 65wt%, O is 0.05 ~ 25wt%, H is 2wt
% Or less, and substantially an amorphous material composed of Si, C and O, or a carbonized material composed of a crystalline aggregate of β-SiC and an amorphous SiO _{2 of} 1000 ° or less. Silicon fiber.

Further, the present invention provides the above-mentioned fastening member, wherein the inorganic long fiber is a silicon nitride-based fiber of the following (4). (4) Si, N, O, C, H, and metals (at least one selected from the group of metal elements of Groups II to VIII of the Periodic Table of the Elements), and the ratio of each element is atomic N / Si = 0.3-3 O / Si = 15 or less C / Si = 7 or less H / Si = 1 or less Metals / Si = 5 or less and the X-ray small-angle scattering intensity ratio is expressed as a ratio. A silicon nitride-based fiber that is 1 to 20 times at 1 ° and 0.5 °, respectively.

Further, the present invention provides the above-mentioned fastening member, wherein the inorganic long fiber is an alumina-based fiber of the following (5). (5) Alumina fibers which are aggregates of mullite and / or γ-alumina and η-alumina microcrystals and amorphous SiO ₂ substantially consisting of Al, Si, B and O.

Further, according to the present invention, the glass ceramic has a main crystal phase of celsian (SrO (and / or BaO) .Al ₂ O ₃ .2SiO ₂ ) and barium osmilite (BaO.2MgO.3Al ₂ O _3. 9Si
O ₂ ) or cordierite (2MgO · 2Al ₂ O ₃₎
.5SiO ₂ ).

Further, according to the present invention, the fastening member comprises a main body, and a peripheral surface layer formed on an outer peripheral surface or an inner peripheral surface of the main body and forming a thread. Are provided in the axial direction of the fastening member, and in the peripheral surface layer, the inorganic long fibers are provided at a predetermined angle with respect to the axial direction of the fastening member. Is what you do.

[0018]

BEST MODE FOR CARRYING OUT THE INVENTION The fastening member of the present invention will be described below in more detail. The fastening member of the present invention is made of a composite material of a specific inorganic long fiber and a specific glass ceramic.

The inorganic long fibers used in the present invention include:
A material used as a reinforcing material in a composite material,
In the present invention, it is a silicon carbide fiber, a silicon nitride fiber, or an alumina fiber. The inorganic long fiber is not particularly limited as long as it is the above-mentioned silicon carbide fiber, silicon nitride fiber or alumina fiber, but the following (1)
The fibers (5) to (5) are preferably used. In use, these may be used as a mixture.

(1) Substantially Si, Ti and / or Z
amorphous consisting of r, C, and O;
0 ° or less, preferably 10 to 100 ° β-SiC,
A crystalline aggregate of TiC and / or ZrC, or an amorphous mixed system composed of TiOx and / or ZrOx (0 <x ≦ 2); And the elemental composition is that Si is 45-60 wt.
%, Ti and / or Zr are 0.2-5 wt%, and C is 20%
A silicon carbide-based fiber having a content of O to 45 wt% and O of 0.1 to 20.0 wt%.

(2) The element composition is such that Si is 30 to 80 wt.
%, C is 20 to 70 wt%, H is 2 wt% or less, preferably 0.5 wt% or less (H is preferably 0 wt%, but may be mixed in the manufacturing process). And an amorphous phase substantially composed of Si and C and / or β of 10000 ° or less, preferably 10 to 2000 °.
A silicon carbide-based fiber composed of crystalline SiC and carbon aggregates. The silicon carbide fiber (2) may be obtained by a CVD method using a normal carbon fiber or tungsten fiber as a core wire.

(3) The element composition is such that Si is 30 to 80 wt.
%, C is 10 to 65 wt%, O is 0.05 to 25 wt%
%, H is 2 wt% or less, preferably 0.5 wt% or less (H is preferably 0 wt%, but may be mixed in the manufacturing process), and substantially contains Si. , C and O, or 1000 ° or less, preferably 0.1 to 200 °, more preferably 10 ° or less.
Crystalline aggregate of β-SiC and amorphous S
A silicon carbide fiber which is an aggregate made of iO ₂ .

(4) Si, N, O, C, H, and metals (at least one selected from the group of metal elements of Groups II to VIII of the periodic table). The ratio is expressed as an atomic ratio. N / Si = 0.3 to 30 / Si = 15, preferably 0.01 to 1 C / Si = 7 or less, preferably 0.01 to 1 H / Si = 1 or less , Preferably 0.01 to 0.2 metals / Si = 5 or less, preferably 0.01 to 0.1, and the X-ray small-angle disturbance intensity ratio is 1 ° and 0.5 °.
1 to 20 times each.

(5) Alumina fibers which are an aggregate of microcrystals of mullite consisting essentially of A1, Si, B, and 0 and / or microcrystals of γ-alumina and -alumina and amorphous SiO ₂ .

Here, the term "in the vicinity" of the above-mentioned fiber (1) is preferably a region whose distance from the crystalline particles is 100 nm or less. The “carbon aggregate” in the above (2) means that there are a plurality of crystalline and / or amorphous carbon particles having a size of 1000 ° or less. In addition, the above (3)
In "crystalline aggregate" is 0.1 to 1000 μm
m means a set of crystals having a size of m, and “an aggregate composed of crystalline aggregates and amorphous SiO ₂ ” means a size of 0.1 to 1000 μm. Means a plurality of amorphous SiO ₂ particles aggregated in the vicinity of the aggregate of crystals having the same meaning (synonymous with “the vicinity thereof” above), and a plurality of amorphous SiO ₂ particles further aggregated. Note that the number of crystals to be assembled is not limited. Specific examples of the metals used in the above (4) include aluminum, titanium, and zirconium.

The X-ray small-angle scattering intensity ratio was measured as follows. "RJ-200B" manufactured by Rigaku Corporation
Connect a PSPC (Position Detection Proportional Counter) -5 to the "type", and use a tube voltage of 45 KV, a tube current of 95 mA, first and second slits of 0.2 mmφ and 0.15 mmφ respectively, and 0.02 ° The scattering intensity was measured every 1000 seconds. As a sample, a fiber having a length of 15 mm was used.
Use 18mg cut out, length 10mm x width 4m
The measurement was carried out with the film stuck uniformly in the slit of m. The intensity ratio was calculated by comparing with the air scattering intensity at 1 ° and 0.5 °.

As the inorganic long fibers, Ube Industries, Ltd.
Inorganic long fibers made of Si-Ti and / or Zr-CO commercially available as "Tyranno Fiber" (registered trademark) from Nippon Carbon Co., Ltd. Inorganic filaments made of Si—C—O commercially available as “Nicalon” (registered trademark) or “Hinicalon” (registered trademark) (specific examples of the silicon carbide-based fiber (3)); Commercially available products such as inorganic long fibers of the SCS series [specific examples of the above-mentioned silicon carbide fiber (2)] can also be used,
Alternatively, inorganic long fibers substantially consisting of Si, C, O and B [specific examples of the silicon carbide fiber (2)] described in US Pat. No. 5,366,943 may be used. it can. Al ₂ O ₃ fiber (manufactured by DuPont)
3M, Sumitomo Chemical Co., Ltd., etc.) [Specific examples of the alumina-based fiber (5)], Si-CN-based fiber [“HP
Z fiber "(trade name, manufactured by Dow Corning Co.) [Specific examples of the silicon nitride-based fiber (4)], Si ₃ N ₄ fibers (manufactured by Tonen Corp.) [specific examples of the silicon nitride-based fiber (4)] Etc. can also be used.

Further, the fiber diameter of the inorganic long fiber is from 1 to 1
It is preferably 000 μm. The fiber length of the inorganic long fiber is preferably longer than 100 μm.

There is no particular limitation on the form of use of the inorganic long fibers as a reinforcing material, and they can be used as continuous fibers, etc., and are woven from continuous fibers, plain weave, satin weave, multiaxial weave, three-dimensional weave, or The continuous fibers may be used as a sheet-like material that is aligned in one direction, or may be used in a form in which two or more of these are mixed (for example, a form in which the sheet-like materials are stacked).

In the composite material forming the fastening member of the present invention, the above-mentioned glass ceramic is present around the inorganic filaments formed as described above (gap between the inorganic filaments).

The glass ceramic used in the present invention is a material constituting a matrix in the composite material.
₂ 0 _3, SiO _2, SrO and / or glass ceramics containing BaO as essential components, i.e., a glass ceramic having at least one of these four molecules, is easily formed in the glassy state, and the heat resistance by heat treatment A higher crystalline phase is precipitated. Further, the glass ceramic may further contain MgO.
When MgO is contained, the content is preferably 0.1 to 10% by weight based on the entire glass ceramic.

A glass-ceramic compact having such a glass-ceramic is prepared by first producing a glass powder having the same composition as a desired crystal component, and pressing it at a temperature higher than the glass transition point to obtain an arbitrary shape. Thereafter, a desired crystal phase is precipitated by heat treatment to improve heat resistance. Further, it is also possible to pour the molten raw material glass into a molding die and precipitate a desired crystal phase in a cooling process to obtain a molded body. And, the composite material is an inorganic long fiber reinforced composite material (hereinafter, referred to as a glass ceramic matrix).
(Hereinafter referred to as "GMC"), it is dense and has almost no pores unlike other long fiber reinforced composite materials such as C / C composite materials. It is also known that GMC maintains high strength from room temperature to high temperature and has high toughness (K.
M. Prewo et al. Mater. Sci. , 17 [1
2] P3549-3563). Further, the processing is easier than that of general monolithic ceramics, and since it is dense, the dimensional accuracy can be kept higher than that of a C / C composite material.

The composition of the glass ceramic is not particularly limited as long as it contains each of the above components. However, as the main crystal phase, celsian (monoclinic celsian) [SrO (and / or BaO) .Al ₂ O _3. 2SiO ₂ ), barium osmilite (BaO
2MgO ・ 3Al ₂ O ₃・ 9SiO ₂ ) or cordierite (2MgO ・ 2Al
_It is preferable to have ₂ O ₃ · 5SiO ₂ ). The celsian, the barium osmilite, and the cordierite can each be used alone or in combination of two or more, and are contained as an aggregate of one or more of these crystals. is there. Further, the glass ceramic may be formed only by the aggregate of the above crystals (that is, at 100 wt% of the aggregate), but the aggregate of the above crystals is at least 50 wt%, preferably 80 wt% or more.
Preferably, it is contained in an amount of about 100% by weight. When mixed with other components, components usually used for glass ceramics can be used without any particular limitation. Here, the “crystal aggregate” is 0.1 to 1000 μm.
It means that a plurality of crystals having a size of m are aggregated, and the number of aggregated crystals is not limited. If the content of the crystal aggregate is less than 50 wt%, the obtained fastening member may not have the required mechanical properties such as heat resistance and bending strength. Is preferred.

The glass ceramics described above include Zr
An element belonging to Group 4A of the periodic table, such as the element, can also be added as a nucleating agent. These elements may be used in any form, but are preferably used in the form of an oxide such as ZrO ₂ . In addition, the amount of the nucleating agent added,
For example, when used as an oxide, the content is preferably 10% by weight or less based on the entire glass ceramic,
More preferably, it is 0.1 to 10% by weight.

In the fastening member of the present invention, the mixing ratio of the inorganic long fiber and the glass ceramic is as follows:
Although there is no particular limitation, the content of the inorganic long fibers is 30 vol.
It is preferable that the content of the glass ceramic is 70 vol% to 30 vol%.
%). When the content of the inorganic long fiber is less than 30 vol%, the effect of the reinforcing fiber is small when processed as a fastening member, and the required mechanical strength may not be maintained, and the fiber content is 70 vol%. If it exceeds, there will be too many places where the inorganic long fibers directly contact each other,
This becomes a large defect, and the fastening member obtained by processing often does not exhibit sufficient mechanical strength, which is not preferable.

The orientation of the inorganic filaments in the fastening member of the present invention is not particularly limited. However, in order to enhance the reinforcing effect of the inorganic filaments, as described below,
It is preferable to have a structure composed of a main body oriented in the axial direction and a peripheral layer oriented at an angle to the axial direction.

Hereinafter, preferred embodiments of the fastening member of the present invention will be described in detail with reference to the drawings. Here, FIG. 1 is a perspective view showing a bolt as a fastening member of the present invention,
FIG. 2A is an enlarged sectional view taken along line AA of FIG.
(B) is a BB enlarged sectional view of FIG. 1, and FIG. 3 is a plan view showing a peripheral surface layer of the fastening member shown in FIG. FIG. 4A is a cross-sectional view illustrating another form of the AA section of the fastening member illustrated in FIG. 1, and FIG. 4B is a cross-sectional view of the fastening member illustrated in FIG. FIG. 5 is a perspective view showing a peripheral surface layer of the fastening member shown in FIG. 2 and 4, screw threads are omitted for easy understanding of the internal structure of the fastening member of the present invention.

The bolt 1 as a fastening member of the present embodiment is
As shown in FIGS. 1 to 3, it is composed of inorganic long fibers 2 as a reinforcing material and glass ceramics 3 as a matrix. To describe this embodiment in more detail, the bolt 1
As shown in FIG. 1, it is composed of a bolt head 1A and a screw portion 1B, and has the same outer shape as a normal bolt. Then, as shown in FIGS. 2A and 2B, the bolt 1 of this embodiment
A main body 10 and a peripheral surface layer 20 which is located on the outer peripheral surface of the main body 10 and forms a screw thread. In the main body 10, the inorganic long fibers 2 are disposed in the axial direction D of the bolt 1 as a fastening member.
In the peripheral layer 20, the inorganic long fibers 2 are disposed at a predetermined angle θ ゜ with respect to the axial direction D of the bolt 1 as a fastening member, as shown in FIGS. (See FIG. 3). Here, having an angle θ ゜ with respect to the axial direction of the main body is an angle when the axial direction D of the bolt is 0 ° as shown in FIG. 3, and in the present embodiment, the axial direction D Is + θ 場合 when tilted counterclockwise with respect to the left direction, and −θ ゜ when tilted θ ° so as to face the opposite direction.

More specifically, the main body 10 shown in FIG.
As shown in (A) and (B), a plurality of the inorganic long fibers 2 are arranged in the form of continuous fibers at predetermined intervals in the axial direction D of the bolt 1 at a predetermined interval. . Also,
As shown in FIG. 2A, the diameter L is preferably 10% or more, more preferably 30% to 90% of the root diameter of the screw of the bolt 1. is there. If the diameter is less than 10%, the ratio contributing to the tensile strength of the bolt is too small, and the mechanical properties thereof do not reach the required level. On the other hand, when the diameter exceeds 90%, the distance between the root of the screw and the outer surface of the main body is too short, and when a stress is applied to the screw thread, the crack of the screw thread reaches the main body. Does not reach the required strength level.

The peripheral surface layer 20 includes a plurality of alignment layers 21, 22, 2, each having a different orientation direction of the inorganic long fiber.
1 ', 22',..., 20n, 20n 'are laminated. The orientation layer will be described with reference to FIG.
As shown in (A) and (B), each alignment layer 21, 21 ′
.. Indicate that the alignment layer 21 and the alignment layer 21 ′ are overlapped with each other so as to cover the peripheral surface of the main body 10 and divide the bolt 1 into an upper surface side and a lower surface side. 20n are sequentially laminated on the alignment layer 21, and the alignment layers 22 ',.
n ′ are stacked. Thus, an orientation layer is arranged in point symmetry above and below. Also, as shown in FIG. 3, each of the alignment layers 21, 22,... Has a flat plate shape in which a central portion in the width direction is protruded toward the axial direction of the bolt. Further, in the present embodiment, the alignment layer 20n which is the outermost layer of the peripheral layer 20 is formed.
Is a plate-like layer having an arc-shaped cross section, as shown in FIG.

Then, each of the alignment layers 21, 21 ', 22, 2
In 2 ′, the inorganic long fibers are arranged at predetermined intervals and at predetermined angles, as shown in FIGS. Further, the alignment layer 21 and the alignment layer 21 ′ are respectively
The orientation layers 22 and 22 'are arranged at the same angle-[theta] (not shown). Thus, the alignment layer 21 is
As an n-th layer, an n-th layer above the alignment layer 21 and an alignment layer 21 ′ as a first layer, the alignment layer 2
It is preferable that the inorganic long fibers are arranged at the same angle with the n-th layer below 1 ′. still,
The terms "upper" and "lower" refer to the upper side of the main body as upper and the lower side as lower in the drawings for convenience of description. The number of layers of the alignment layers in the peripheral layer 20 is relatively determined from the root diameter and the peak diameter of the target screw and the thickness of the alignment layer made of each composite material. The thickness of each of the alignment layers is preferably 20 to 400 μm.

The orientation layer 21 (21 ') has an angle of + θ °, and the second orientation layer 22 (22') has an angle of -θ °.
Thus, the inorganic long fibers 2 are provided. That is, in the present embodiment, layers at angles + θ and layers at −θ are alternately arranged. Here, the angle θ is preferably 5 ° <θ ≦ 60 °, and more preferably 30 ° <θ ≦ 60 °. If the angle θ is less than 5 °, there is no or very little reinforcing effect by the reinforcing fiber in the direction perpendicular to the bolt axis direction. . That is, a problem that workability is deteriorated occurs, which is not preferable. Also, even if threading can be performed, this thread has an effect of fiber reinforcement only for simple tension in the axial direction, and the thread easily separates when fitted with a nut and subjected to stress. As a result, the required mechanical strength cannot be realized, which is not preferable. Further, when θ exceeds 60 °, thread processing is relatively easy, but the reinforcing effect in the bolt axis direction on the main body is very small, and the difference in fiber orientation angle between the main body and the peripheral layer is large. When a stress is applied by fitting with the nut, a crack is generated between the main body and the peripheral surface layer, and the main body and the peripheral surface layer come off from each other, and the required mechanical strength cannot be realized. .

The angle θ of each of the alignment layers can be set as follows. That is, the angle can be sequentially changed from the alignment layer 21 (21 ′) to the alignment layer 20n (20n ′). For example, the angle of the alignment layer 21 (21 ') is set to +
and theta _1, the alignment layer 22 (22 ') the angle of the case of the - [theta] _1, the alignment layer 20n over 1 (20n-1' is the angle of) +
In each alignment layer, the angle can be increased by α ° so that the angle is 60 ° and the angle of the alignment layer 20n (20n ′) is −60 °. Here, θ ₁ is 0 <θ
₁ ≦ 60 ° and α are arbitrary values of 0 <α ≦ 60 °, but preferably 0 <θ ₁ ≦ 5 ° and 0 <α ≦ 5 °. If theta ₁ is greater than 5 °, to the difference between the fiber-reinforced direction of the main body and the peripheral surface layer increases, the easy peeling occurred in this area when stress is applied to the screw is not preferable. On the other hand, when α exceeds 5 °, the difference in the direction of fiber reinforcement per layer of the peripheral layer increases, so that separation between the layers tends to occur, and the required mechanical strength cannot be realized. Absent.

Therefore, for example, when θ ₁ is 5 ° and α is 5 °, the alignment layers 22 (22 ') and 20n
-1 (20n-1 '), ± 10 °, ± 15
゜, ± 20 ゜, ± 25 ゜, ± 30 ゜, ± 35 ゜, ± 40
゜, ± 45 ゜, ± 50 ゜, ± 55 ゜ total 20 ×
There will be two layers (ie there are a total of 48 alignment layers).

The density of the inorganic filaments 2 in the main body 10 is preferably 2.1 to 4.9 g / cm ^3, and the length is preferably equal to the length of a fastening member (bolt). The fiber diameter is preferably 5 to 200 μm. The density of the glass ceramics 3 is 2.2 to 2.2.
It is preferably 3.8 g / cm ³ . The density of the inorganic long fibers 2 in the peripheral layer 20 is 2.1 to 4.0.
It is preferable to be 9 g / cm ^3, length of 20 times the length and circumference of the length of the crest diameter of the thread of the circumferential length of 1/20 to the fastening member of the crest diameter of the thread length And the fiber diameter is preferably 5 to 200 μm. The density of the glass ceramics 3 is 2.2
It is preferable to set it to 3.8 g / cm ³ .

Next, another embodiment of the fastening member of the present invention will be described with reference to FIGS. Note that, for the points that are not particularly described in detail, the description given in the embodiment shown in FIGS. As shown in FIGS. 4A and 4B, the bolt 1 as a fastening member having the form shown in FIGS. 4 and 5 includes an inorganic long fiber 2 as a reinforcing material and a glass ceramic 3 as a matrix.
As shown in FIGS. 4A and 4B, the bolt 1 includes a round bar-shaped main body 10 and a peripheral layer 20 located on the outer peripheral surface of the main body 10 and forming a thread. Further, as shown in FIGS. 4B and 5, the peripheral surface layer 20 includes cylindrical alignment layers 21, 22,..., 20n. Each of the alignment layers 21, 22,...
As shown in the figure, the inorganic long fibers 2 are cylindrical and spirally arranged. The inorganic long fibers 2 are arranged at an angle of + θ in the alignment layer 21.
In 2, the inorganic long fibers 2 are arranged at an angle -θ. As described above, in the present embodiment, the orientation layers in which the inorganic long fibers are arranged at an angle of + θ and the orientation layers in which the inorganic long fibers are arranged at an angle of -θ are alternately arranged. The description given in the above-described embodiments shown in FIGS. 2 and 3 is applied to the density and the fiber diameter of the inorganic long fibers and the density of the glass matrix. However, the length of the inorganic long fibers is spirally arranged. It is preferable that the length be as long as possible, and the length is preferably up to about five times the length of the fastening member.

Further, the above-mentioned peripheral layer may be formed as follows. That is, as shown in FIG. 6, the upper alignment layers 21, 22,...
.20n and lower alignment layers 21 ', 22'... 20n '
20n and the lower alignment layers 21 ′, 22 ′... 20n ′ may form a cylindrical alignment layer.

As described above, the fastening member of the present invention is composed of inorganic long fibers and glass ceramics, and therefore has a dense structure and is excellent in various strengths.
Furthermore, it has excellent heat resistance and environmental resistance. Here, "dense" means that there are substantially no pores or the like in the matrix, and specifically, that the apparent density is 95% or more of the theoretical density.

In the above description, the bolt has been exemplified, but the structure of the fastening member of the present invention can be applied to a nut. At this time, in the nut, the axial direction is the same as the axial direction of the bolt (the direction of the center of the inner circumference of the nut), and the peripheral surface layer is a peripheral surface that forms a thread on the internal peripheral surface of the bolt. In the case of a nut,
Inorganic long fiber is a two-way reinforced laminate obtained by alternately laminating prepreg sheets arranged in an O ° direction and prepreg sheets arranged in a 90 ° direction, wherein the two-way reinforced laminate is a nut shaft. Machine the screw holes to be in the direction,
May be produced.

Next, a method for manufacturing the fastening member of the present invention will be described. The fastening member of the present invention can be obtained by preparing a fiber-reinforced base material using the inorganic long fibers and the glass ceramics according to a conventional method, and then forming the bolt into any desired shape by mechanical processing. .

Further, a fastening member having a main body and a peripheral layer in which the orientation direction of the inorganic long fiber is different from the main body, such as the bolt having the form shown in FIG. 2, is preferably formed by the following method i). ii) and the like. i) A method of forming a composite round bar to be a main body, and then forming a peripheral layer on the peripheral surface of the round bar (for manufacturing a bolt having the form shown in FIGS. 2 and 3 and a bolt shown in FIG. 6). Preferred method). ii) A method of simultaneously forming the main body and the peripheral surface layer (a method suitable for manufacturing a bolt having the form shown in FIGS. 4 and 5).

The method i) will be described in detail. In the method i), first, a round bar constituting the main body is manufactured. Next, a laminate of prepreg sheets comprising inorganic filaments, a matrix powder, and an organic binder for adhering them to each other was arranged above and below the round bar so as to have a desired peripheral layer structure. With the device,
The substrate is obtained by hot pressing in a pseudo-isotropic manner, followed by further heat treatment. The hot press device shown in FIG. 7 will be described in detail. The hot press 30 shown in FIG. 7 is the same as a known hot press device, and includes an upper punch rod 31, a lower punch rod 32, and an upper punch rod 31. And a die 33 for supporting the lower punch rod 32, and a pressure medium powder 34 made of graphite powder and the like disposed below the upper punch rod 31 and above the lower punch rod 32, respectively. Pressing can be performed by sandwiching a plurality of the inorganic long fiber preforms (prepreg sheets) between the non-woven fabrics 34. Here, "pseudo-isotropic" means that an inorganic powder that is not sintered under the molding conditions in this manufacturing method, such as a carbon powder, is placed around a hot-pressed preform as shown in FIG. This means that hot press is performed using this as a pressure medium to form a deformed material. Then, the obtained base material is finished into an arbitrary bolt shape by ordinary machining to obtain a desired fastening member.

The above-mentioned round bar is prepared by adhering matrix raw material powder to the surface of inorganic long fibers, producing a sheet-like material aligned in one direction, laminating a large number of sheets in the same direction, and using an apparatus shown in FIG. Hot pressing, and then heat treatment to obtain a flat plate. Then, the obtained flat plate can be obtained by machining. The hot pressing is preferably performed at a pressure of 0.1 to 20 MPa, a pressing time of 5 to 60 minutes, and a temperature of 800 to 1100 ° C. The conditions of the heat treatment are 1100 to 1400 ° C.
And preferably for 1 to 24 hours. Further, it is preferable that the heat treatment is performed immediately after the end of the hot pressing.

The hot pressing of the round bar and the prepreg sheet will be described with reference to FIG. 8. Referring to FIG. 8, flat prepreg sheets 21A, 21A ', 22A and 22A' are provided above and below the obtained round bar-shaped main body, respectively. .. Are arranged in a desired number, and the upper and lower punch rods 31 and 32 are
By performing the pressing in the direction of the arrow, the pseudo isotropic hot pressing can be performed via the pressure medium powder 34. Then, by variously changing the orientation direction of the inorganic long fibers in the prepreg sheet, the angle θ in each orientation layer can be variously changed. Also, by adjusting the width of the prepreg sheet, FIG.
3 and the form shown in FIG. 6.

The conditions for hot pressing the main body and the laminate of the prepreg sheet are as follows:
0 MPa, pressurizing time 5 to 60 minutes, temperature 8
The temperature is preferably from 100 to 1100 ° C. The heat treatment is preferably performed at 1100 to 1400 ° C. for 1 to 24 hours. Further, it is preferable that the heat treatment is performed immediately after the end of the hot pressing.

Next, the method ii) will be described in detail. First, in the method ii), a preform suitable for an intended fastening member (bolt), that is, the above-mentioned round bar-shaped main body and the cylindrical above-mentioned main body are used. An inorganic long fiber preform in which inorganic long fibers are arranged at a predetermined angle so as to form a peripheral layer is manufactured. Next, the inorganic long fiber preform is set in a usual mold, a molten matrix material is poured, and a desired glass ceramic crystal phase is precipitated in a cooling process to obtain a base material. The obtained base material is finished into a desired shape such as an arbitrary bolt shape by machining to obtain the fastening member of the present invention.

The inorganic long fiber preform is such that the inorganic long fibers aligned in one direction are disposed at the center, and the fibers are spirally wound around the outside thereof, and the winding direction is changed for each layer. It can be manufactured by At this time, it is preferable that the inorganic long fiber preform is solidified by an organic binder and kept in shape. The fiber preform is placed at a predetermined position on the bottom of a graphite die coated with a release agent so as not to react with the matrix at a high temperature, and the upper portion is filled with a matrix raw material powder. Then, the dies are heated to dissolve the matrix glass and permeate the fiber preform. At this time, it is preferable to use a hot press device having a die as shown in FIG. 9 and pressurize in a short time so that the permeation is performed in a short time so as not to generate voids.

The hot press apparatus shown in FIG. 9 will be described in detail. The hot press 50 shown in FIG. 9 is the same as a known hot press apparatus.
A lower punch rod 52 having a groove 54 for setting a preform, an upper punch rod 51 and a die 53 for supporting the lower punch rod 52 are provided.
By setting a fiber preform in 4 and holding a matrix powder between the fiber preform and the upper punch rod 51, pressurization can be performed.

When hot pressing is performed by using the above hot pressing apparatus, the pressure is preferably 5 to 30 MPa, the pressing time is preferably 2 to 10 minutes, and the temperature is 1400 to 1600 ° C. Is preferred.

Thereafter, a heat treatment is carried out in a temperature lowering process to precipitate a desired glass-ceramic phase in the matrix glass. The conditions of the heat treatment are 1000 to 14
It is preferable to set the temperature at 00 ° C. for 1 to 24 hours. The heat treatment is preferably performed after the temperature is once raised to 1000 ° C.

Then, the obtained base material is subjected to ordinary machining to obtain a desired shape such as a bolt shape, whereby the fastening member of the present invention can be obtained.

[0062]

EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples, but the present invention is not limited to these examples.

<Example 1> Inorganic long fiber [Si-Ti-C
-O fiber, manufactured by Ube Industries, Ltd., trade name "Tyranno Fiber F
Lade ”] and glass ceramic powder (SrO
-MgO-Al_TwoO _Three-SiO_Two, Compounding ratio (SrO: M
gO: Al_TwoO_Three: SiO_Two= 18: 4: 28: 50)
2500 g of 8000 g of water and an organic binder (polyethylene)
Lenoxide) in a dispersion medium consisting of 500 g
Impregnated by impregnating, winding and drying
This produced a one-way prepreg sheet.

The obtained prepreg sheets were laminated to obtain a laminate. The prepreg sheets were laminated with the fiber orientation direction being the same. The obtained laminate was
By hot-pressing at 00 ° C. for 20 minutes at 10 MPa and further performing heat treatment at 1300 ° C. for 1 hour to perform crystallization, a thick plate of a fiber-reinforced composite material having fibers oriented in one direction was produced. Using the obtained thick plate, a round bar of φ4 mm × L50 mm was processed so that the fibers were oriented in the longitudinal direction. + 5 ° to +60 on the obtained round bar. And a total of 24 prepreg sheets (each having a thickness of 200 μm) inclined at an orientation angle of 5 ° from −5 ° to −60 ° in increments of 5 °
Were laminated so that layers having an angle of-and layers having an angle of-were alternately laminated to obtain a preform.

This preform was placed inside a graphite die shown in FIG. 7, and carbon powder was charged above and below it.
Hot pressing at 1000 ° C. for 1 hour and pseudo-isotropic at 10 MPa, followed by heat treatment at 1300 ° C. for 1 hour for crystallization to obtain a dense compact, which was used as a screw base. This screw base is machined and
An M10 screw composed of a main body shown in Fig. 7 and a peripheral surface layer composed of 24 orientation layers disposed on the peripheral surface of the main body was obtained.

The obtained M10 screw had a tensile strength at room temperature of 380 MPa and a tensile strength in air at 1000 ° C. of 350 MPa.

<Example 2> Inorganic long fiber [Si-Ti-C
-O fiber, manufactured by Tanabe Kosan Co., Ltd. under the trade name "Tyranno slow fiber F grade"], and glass ceramic powder (BaO
—MgO—Al ₂ O ₃ —SiO ₂ , mixing ratio BaO: Mg
O: Al ₂ O ₃ : SiO ₂ = 14: 8: 28: 50) 2
700 g was immersed and impregnated in a slurry dispersed in a dispersion medium consisting of 8000 g of water and 270 g of an organic binder (polyethylene oxide), wound up, and dried to produce a unidirectional prepreg sheet.

The obtained prepreg sheets were laminated to obtain a laminate. The prepreg sheets were laminated with the fiber orientation direction being the same. The obtained laminate was
By hot-pressing at 10 MPa for 30 minutes at 00 ° C., and further performing heat treatment at 1300 ° C. for 1 hour to perform crystallization, a slab of fiber-reinforced composite material having fibers oriented in one direction was obtained. . Using the obtained thick plate, a round bar of φ5 mm × L50 mm was processed so that the fibers were oriented in the longitudinal direction. From the obtained round bar to + 5 ° to + 60 °, and-
A total of 24 prepreg sheets (thickness: 300 μm) each having an inclination angle of 5 ° to −60 ° in increments of 5 ° are laminated so that layers having a positive angle and layers having a negative angle are alternately laminated. And
It was a preform.

This preform was placed inside a graphite die shown in FIG. 7, and carbon powder was filled above and below the preform.
Hot pressing at 1000 ° C. for 1 hour and pseudo-isotropic at 10 MPa, followed by heat treatment at 1300 ° C. for 1 hour for crystallization to obtain a dense compact, which was used as a screw base. This screw base is machined and
An M10 screw composed of a main body shown in Fig. 7 and a peripheral layer composed of an orientation layer of 24 eyebrows arranged on the peripheral surface of the main body was obtained. M obtained
10 screws had a tensile strength at room temperature of 320 MPa and 1
The tensile strength in air at 000 ° C. was 300 MPa.

<Example 3> A silicon carbide fiber (trade name “Nicalon” manufactured by Nippon Carbon Co., Ltd.) was opened, and a glass ceramic powder (BaO—MgO—Al ₂ O ₃ —SiO) was opened.
₂ , compounding ratio BaO: MgO: Al ₂ O ₃ : SiO ₂ = 1
5: 4: 29: 52) and a silicon carbide powder mixed at a weight ratio of 6: 1, 3500 g of a mixture, 5000 g of water, 3000 g of ethanol and 400 g of an organic binder (polyvinyl alcohol) dispersed in a dispersion medium comprising a dispersion medium. To obtain a unidirectional prepreg sheet by impregnating, winding and drying.

The obtained prepreg sheets were laminated to obtain a laminate. The prepreg sheets were laminated with the fiber orientation direction being the same. The obtained laminate was
By hot-pressing at 00 ° C. for 1 hour and 10 MPa, and further performing heat treatment at 1300 ° C. for 1 hour to perform crystallization, a thick plate of a fiber-reinforced composite material having fibers oriented in one direction was produced. Using the obtained thick plate, a round bar of φ5 mm × L50 mm was processed so that the fibers were oriented in the longitudinal direction. From + 7.5 ° to + 60 ° on the obtained round bar,
In addition, a total of 16 prepreg sheets (each having a thickness of 250 μm) in which the orientation angle was inclined from −7.5 ° to −60 ° in increments of 7.5 °.
m) was laminated so that layers with a positive angle and layers with a negative angle were alternately laminated to obtain a preform.

This preform was placed inside a graphite die shown in FIG. 7, and carbon powder was filled above and below the preform.
Hot pressing at 1000 ° C. for 1 hour and pseudo-isotropic at 10 MPa, followed by heat treatment at 1300 ° C. for 1 hour for crystallization to obtain a dense compact, which was used as a screw base. This screw base is machined and
An M10 screw composed of the main body shown in Fig. 7 and a peripheral surface layer composed of 16 orientation layers disposed on the peripheral surface of the main body was obtained. M obtained
The ten screws had a room temperature tensile strength of 200 MPa. The tensile strength in air at 1000 ° C is 180M
Pa.

<Example 4> As an inorganic long fiber, one composed of a microcrystalline aggregate having the following composition was used. Composition: S
i, N, C, O and H, and the internal element composition is S
i: 59.2 wt%, N: 37.5 wt%, C: 1.5
wt%, O: 1.5 wt%, H: 0.3 wt%,
An aggregate of microcrystals whose main microcrystal is Si ₃ N ₄ of 2000 ° or less. The filaments having the above composition and having a fiber diameter of 10 to 20 µm are sized with 0.5 to 1 wt% of polyvinyl alcohol to form a filament bundle of inorganic filaments of 200 filaments / yarn. Of the glass ceramic powder (B
_{aO-MgO-Al 2 O 3} -SiO 2, mixing ratio BaO:
MgO: Al ₂ O ₃ : SiO ₂ = 14: 8: 28: 5
0) A unidirectional prepreg sheet was manufactured by impregnating a slurry dispersed in a dispersion medium composed of 2600 g, 8000 g of water and 450 g of an organic binder (polyethylene oxide), winding and drying.

The obtained prepreg sheets were laminated to obtain a laminate. The prepreg sheets were laminated with the fiber orientation direction being the same. The obtained laminate was
Hot pressing was performed at 00 ° C. for 30 minutes at 10 MPa, and heat treatment was further performed at 1300 ° C. for 1 hour for crystallization to produce a thick plate of a unidirectional fiber reinforced composite material. Using the obtained thick plate, so that the fibers are oriented in the longitudinal direction,
A round bar of φ5 mm × L50 mm was processed. A prepreg sheet having an orientation angle of + 60 ° and -6
A preform was formed by laminating 16 preg sheets (each having a thickness of 200 μm) having an orientation angle of 0 ° such that layers having a positive angle and layers having a negative angle were alternately laminated. .

This preform was placed inside a graphite die shown in FIG. 7, and carbon powder was filled above and below it.
Hot pressing at 1000 ° C. for 1 hour and pseudo-isotropic at 10 MPa, followed by heat treatment at 1300 ° C. for 1 hour for crystallization to obtain a dense compact, which was used as a screw base. This screw base is machined and
As shown in (1), an M10 screw composed of a main body and a peripheral surface layer composed of two orientation layers disposed on the peripheral surface of the main body was obtained. The obtained M10 screw had a room temperature tensile strength of 220 MPa and a tensile strength in air of 1000 ° C. of 200 MPa.

Example 5 The following composition was used as the inorganic long fiber:
Was used. Composition: A1, Si, B, 0, internal elemental composition
A: 37.1 wt%, Si: 18.1 wt%,
B: O. 6 wt%, O: 44.2 wt%, γ-A
Or an aggregate of microcrystals of η-alumina and amorphous Si
O_TwoAn aggregate consisting of And, having the above composition,
The diameter of the fiber is 10-20 μm.
BN coating, 0.5-1 wt% of polyvinyl chloride
1800 feet sized with nil alcohol
Filament of inorganic filaments in a filament / yarn fiber bundle
The filament assembly is opened and the glass ceramic powder is opened.
(BaO-MgO-Al_TwoO_Three-SiO_Two, Compounding ratio Ba
O: MgO: Al_TwoO_Three: SiO _Two= 14: 8: 28:
50) and silicon carbide powder mixed at a weight ratio of 6: 1
3600 g of water, 6000 g of water and 20 ethanol
00g organic binder (polyvinyl alcohol) 600
impregnated with a slurry dispersed in a dispersion medium consisting of
One-way prepreg by winding, drying and drying
A sheet was manufactured.

The resulting prepreg sheets were laminated to obtain a laminate. The prepreg sheets were laminated with the fiber orientation direction being the same. The obtained laminate was
By hot-pressing at 00 ° C. for 1 hour and 10 MPa, and further performing heat treatment at 1300 ° C. for 1 hour to perform crystallization, a thick plate of a fiber-reinforced composite material having fibers oriented in one direction was produced. Using the obtained thick plate, a round bar of φ5 mm × L50 mm was processed so that the fibers were oriented in the longitudinal direction. On the obtained round bar, a total of 16 prepreg sheets (each having a thickness of 300) were tilted at + 7.5 ° to + 60 ° and at −7.5 ° to −60 ° in 7.5 ° increments.
μm) was laminated so that layers having a positive angle and layers having a negative angle were alternately laminated to obtain a preform.

This preform was placed inside a graphite die shown in FIG. 7, carbon powder was not placed above and below it as a pressure medium, and hot pressed at 1000 ° C. for 1 hour at 10 MPa in a pseudo isotropic manner. By performing a heat treatment at 1300 ° C. for 1 hour to perform crystallization, a dense compact is obtained,
This was used as a screw substrate. This screw base material was machined to obtain an M10 screw composed of the main body shown in FIGS. 1 to 3 and a peripheral surface layer composed of 16 orientation layers disposed on the peripheral surface of the main body.
The obtained M10 screw has a room temperature tensile strength of 180MP.
a. The tensile strength in air at 1000 ° C. was 170 MPa.

<Example 6> An inorganic long fiber [SiC fiber, manufactured by Textron Co., Ltd., trade name "SCS-6"] was replaced with 2
The pieces were cut to a length of 0 cm and arranged in a row. Glass ceramic powder _{(SrO-MgO-Al 2 O} 3 -Si
O ₂ , compounding ratio (weight ratio, hereinafter the compounding ratios are all by weight) SrO: MgO: Al ₂ O ₃ : SiO ₂ = 18:
4:28:50) 2500 g of a slurry composed of 8000 g of water and 500 g of an organic binder (polyvinyl alcohol) was applied onto the aligned fiber array and dried.
The obtained mat-like sheet was wound into a rod having a diameter of about 5 mm, and a 5% solution of polyvinyl alcohol was applied and dried to prepare a rod-shaped preform. The obtained rod-shaped preform was impregnated with a fiber bundle obtained by impregnating an inorganic long fiber [Si-Ti-CO fiber, manufactured by Ube Industries, Ltd., trade name "Tyranno fiber LoxE grade"] with a 5% polyethylene solution.
The orientation angle is 60 ° with respect to the axial direction of the rod-shaped preform.
Then, after winding up to the end, the layers were turned upside down (the orientation angle was set to −60 °) to alternately form layers of fiber bundles having different orientation directions. This operation was repeated to produce a fiber preform having 26 layers (each having a thickness of 100 μm) and dried. After drying, the fiber preform solidified by the organic binder is 5 cm.
Cut to length.

The cut fiber preform is set in the groove 54 of the lower punch rod 52 shown in FIG. 9, and an appropriate amount of glass ceramic powder (SrO—MgO—Al ₂
O ₃ —SiO ₂ , compounding ratio (SrO: MgO: Al
₂ O ₃ : SiO ₂ = 18: 4: 28: 50)
Set upper punch rod 51, 1500 ℃, 15MPa
After hot-pressing for 10 minutes and cooling to 1000 ° C., heat treatment was again performed at 1300 ° C. for 1 hour to obtain a molded body, which was used as a screw base. This screw base material is machined to form an M having a main body shown in FIGS. 1, 4 and 5 and a peripheral surface layer composed of 26 cylindrical alignment layers disposed on the peripheral surface of the main body.
10 screws were obtained.

The obtained M10 screw had a tensile strength at room temperature of 180 MPa and a tensile strength in air at 1000 ° C. of 160 MPa.

The tensile strengths at room temperature and at 1000 ° C. measured in the above-described examples are measured as follows. That is,
The M10 screw is threaded in the thickness direction of a two-way reinforced laminated board (a sheet in which inorganic long fibers are oriented in a 0 ° direction and a sheet in which a 90 ° direction is oriented) made of the same material. Then, a composite material nut having an outer diameter of 17 m / m square and a height of 8 m / m was fitted, and the distance between the nuts was set to 3 cm. , AL-50kN "manufactured by Minebea) and pulled at a speed of 1 cm / min. The breaking load at this time is a value calculated by calculating the average diameter of the effective diameter and the root diameter of the screw as the diameter of the effective sectional area.

Reference Example 1 Carbon fiber [manufactured by Toray Industries, Inc.
Product name "T300"] and glass ceramic powder
(BaO-MgO-Al_TwoO_Three-SiO2, compounding ratio Ba
O: MgO: Al _TwoO_Three: SiO_Two= 41: 1: 1
0:48) and alumina powder in a weight ratio of 5: 1.
2,000 g of water and an organic bath
Inder (polyethylene oxide) 500g
Impregnated with a slurry dispersed in a dispersion medium
And dried to produce a one-way prepreg sheet.
Built.

The obtained prepreg sheets were laminated to obtain a laminate. The prepreg sheets were laminated with the fiber orientation direction being the same. The obtained laminate was
Hot pressing was performed at 00 ° C. for 1 hour at 10 MPa, and heat treatment was further performed at 1200 ° C. for 30 minutes to perform crystallization, thereby producing a slab of fiber-reinforced composite material in which fibers were oriented in one direction. Using the obtained thick plate, a round bar of φ5 mm × L50 mm was processed so that the fibers were oriented in the longitudinal direction. A prepreg sheet having an orientation angle of + 60 ° and 10 prepreg sheets (each having a thickness of 200 μm) each having an orientation angle of −60 ° are formed on the obtained round bar by a layer having a positive angle and a layer having a negative angle. Were alternately laminated to form a preform.

This preform was placed inside a graphite die shown in FIG. 7, carbon powder was placed above and below it as a pressure medium, hot-pressed at 1000 ° C. for 1 hour and 10 MPa, and heat-treated at 1200 ° C. for 30 minutes. Then, crystallization was performed to obtain a molded body, which was used as a screw base material. This screw base material was machined to obtain an M10 screw having the shape shown in FIGS. Although the obtained M10 screw had a room temperature tensile strength of 180 MPa, it was exposed to air at 1000 ° C.
Was 40 MPa.

[0086]

The fastening member of the present invention has excellent heat resistance,
Furthermore, even when used in an actual use environment such as in the air from room temperature to high temperature, there is little deterioration in mechanical properties over time, and it is excellent in tensile strength, thread part strength and environmental resistance. is there. More specifically, since the fastening member of the present invention is made of a dense GMC material, not only is the thread workability easy, but also defects such as voids that become the starting points of fracture when stress is applied to the screw thread. Is very low and hardly present compared to conventional composite materials. Therefore, the original strength of the material can be exhibited. In addition, since the glass ceramics as the matrix and the inorganic long fibers as the reinforcing material have excellent oxidation resistance, they can be used from room temperature to high temperature in the atmosphere without deterioration in performance.

[Brief description of the drawings]

FIG. 1 is a perspective view of a bolt as one embodiment of a fastening member of the present invention.

FIG. 2A is a cross-sectional view of the fastening member shown in FIG.
FIG. 2B is a cross-sectional view schematically illustrating one mode of the cross section, and FIG.
FIG. 2 is a cross-sectional view schematically showing one mode of a BB cross section of the fastening member shown in FIG. 1.

FIG. 3 is a perspective view showing a peripheral surface layer of the fastening member shown in FIG. 2;

FIG. 4 (A) is an AA diagram of the fastening member shown in FIG. 1;
FIG. 4B is a cross-sectional view showing another form of the cross section, and FIG.
It is sectional drawing which shows other forms of BB cross section of the fastening member shown in FIG.

FIG. 5 is a perspective view showing a peripheral surface layer of the fastening member shown in FIG. 4;

FIG. 6 is a cross-sectional view showing another form of the BB section of the fastening member shown in FIG. 1;

FIG. 7 is a schematic view of an apparatus used for a quasi-isotropic hot press.

FIG. 8 is a schematic diagram showing an outline of a pseudo isotropic hot press.

FIG. 9 is a schematic view of an apparatus used for hot pressing.

FIG. 10 is a perspective view of a conventional bolt.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Bolt (fastening member) 2 Inorganic long fiber 3 Glass ceramic 10 Main body 20 Peripheral layer 21,22 ... 20n Orientation layer 30 Hot press device 31 Upper punch device 32 Lower punch bar 33 Dice 34 Pressure medium powder (graphite) 35 preforms

 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Takuo Hasegawa 1-1-1 Katase, Fujisawa-shi, Kanagawa Minebea Katase Branch, Advanced Material Utilization Gas Generator Laboratory, Fujisawa Co., Ltd. (72) Inventor, Yukio Shimada 1-1-1 Katase, Fujisawa City, Kanagawa Pref. Minebea Fujisawa Manufacturing Co., Ltd. Advanced Material Use Gas Generator Laboratory Katase Branch Office (72) Inventor Nobuyuki Suzumura 3-12-12 Shinmachi, Hoya City, Tokyo Material utilization gas generator laboratory Tanashiri room

Claims (9)

[Claims] 1. A composite material of an inorganic long fiber and glass ceramic, wherein the inorganic long fiber is at least one selected from the group consisting of a silicon carbide fiber, a silicon nitride fiber and an alumina fiber, the glass _{ceramic, Al 2 0 3, SiO 2} , S
A fastening member comprising glass ceramics containing rO and / or BaO as an essential component. 2. The glass ceramic according to claim 1, further comprising MgO.
The fastening member according to claim 1, further comprising: 3. The fastening member according to claim 1, wherein the inorganic long fiber is a silicon carbide-based fiber of the following (1). (1) Substantially Si, Ti and / or Zr, C,
O and an amorphous phase and β of 500 ° or less.
-A crystalline aggregate of SiC and TiC and / or ZrC, or SiOx present in the crystalline and in the vicinity thereof
And an amorphous mixed system composed of TiOx and / or ZrOx (0 <x ≦ 2), and the elemental composition is as follows:
5-60 wt%, Ti and / or Zr 0.2-5 wt%
%, C is 20 to 45 wt%, and O is 0.1 to 20.0 wt%
% Silicon carbide based fiber. 4. The fastening member according to claim 1, wherein the inorganic long fiber is a silicon carbide fiber described in the following (2). (2) The element composition is such that Si is 30 to 80 wt% and C is 20
70% by weight, H is 2% by weight or less, and amorphous and / or 10,000 substantially composed of Si and C.
(4) A silicon carbide fiber comprising the following β-SiC crystalline and carbon aggregates. 5. The fastening member according to claim 1, wherein the inorganic long fiber is a silicon carbide-based fiber of the following (3). (3) The element composition is such that Si is 30 to 80 wt% and C is 10
~ 65wt%, O is 0.05 ~ 25wt%, H is 2wt
% Or less and substantially consisting of Si, C and O, or 10
Crystalline aggregate of β-SiC of less than 00 ° and amorphous S
A silicon carbide fiber which is an aggregate made of iO ₂ . 6. The fastening member according to claim 1, wherein the inorganic long fiber is a silicon nitride fiber of the following (4). (4) Si, N, O, C, H, and metals (at least one selected from the group of metal elements of Groups II to VIII of the Periodic Table of the Elements), and the ratio of each element is atomic In terms of ratio, N / Si = 0.3-3 O / Si = 15 or less C / Si = 7 or less H / Si = 1 or less Metals / Si = 5 or less, and the X-ray small-angle scattering intensity ratio is 1 each at 1 ゜ and 0.5 ゜
A silicon nitride fiber that is 20 times to 20 times. 7. The fastening member according to claim 1, wherein the inorganic long fiber is an alumina-based fiber of the following (5). (5) Alumina fiber which is an aggregate of microcrystals of γ-alumina and η-alumina and amorphous SiO ₂ substantially consisting of mullite substantially composed of Al, Si, B and O. 8. The glass ceramic has celsian (SrO (and / or BaO) .Al) as its main crystal phase.
₂ O ₃ · 2SiO ₂ ), barium osmilite (BaO)
_2. The fastening member according to claim 1, comprising 2MgO.3Al ₂ O ₃ .9SiO ₂ ) or cordierite (2MgO.2Al ₂ O ₃ .5SiO ₂ ). 9. The fastening member comprises a main body, and a peripheral surface layer which is located on an outer peripheral surface or an inner peripheral surface of the main body and forms a screw thread. The said inorganic long fiber is distribute | arranged toward the axial direction of a member, and in the said peripheral surface layer, the said inorganic long fiber is distribute | arranged at a predetermined angle with respect to the axial direction of a fastening member. Fastening members.