JP3244281B2 - Manufacturing method of jig material for glass container manufacturing - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a jig material for manufacturing a glass container made of carbon fiber reinforced carbon material.

[0002]

2. Description of the Related Art It is well known that glass containers such as glass bottles and glass cups are manufactured by glass forming machines such as IS machines and press machines. The glass container molded by these molding machines is usually 350 to 65 in the transportation process to an annealing layer (annealing furnace).
The temperature is as high as 0 ° C. The glass container in this process,
Due to friction and thermal stress caused by contact with the surface of the jig material for transport, surface cracks called "billi" are apt to enter, and therefore, asbestos and its molded products have conventionally been often used as jig materials for manufacturing glass containers. Recently, since the carcinogenicity of asbestos has attracted attention, graphite materials, heat-resistant plastics, carbon fiber reinforced carbon materials, and the like have begun to be used instead. However, graphite material has high heat resistance, but has the disadvantage that it is inferior in impact resistance and is easily cracked.Also, molded products such as polyimide resin and silicon resin are used as heat-resistant plastics. short.

A carbon fiber reinforced carbon material (also referred to as a C / C composite) is a composite material using carbon fiber as a reinforcing material and carbon as a matrix.
Due to its excellent heat resistance, it has been widely used as a jig material for producing glass containers (for example, Glass).
Technology Vol.26 No.6Dec
member 1985). However, since the conventional C / C composite is manufactured by laminating carbon fiber woven fabrics, there is a drawback that the interlayer shear strength is low and delamination is likely to occur during processing. Therefore, a machine having a large number of holes is provided. It was rarely used for dead plates and take-out tongs that required precise processing. Furthermore, conventional C / C
Composites have low oxidation resistance because they use a non-graphitizable material such as phenolic resin as the matrix.
In addition, when graphite is formed at a high temperature of 2600 ° C. or higher to improve oxidation resistance, the hardness decreases, and when used as a jig material for glass production, the abrasion resistance deteriorates.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to produce a jig material for producing a glass container which has good workability and excellent oxidation resistance and abrasion resistance.

[0005]

SUMMARY OF THE INVENTION According to the present invention, an aqueous dispersion slurry of a raw material containing short fibers of carbon fiber and pitch powder is filtered to form a raw material layer on the surface of a filter medium having a predetermined surface shape. A pre-formed body is formed, and the pre-formed body is compression-molded, and then carbonized to obtain a primary carbonized product.
The product is subjected to one or more impregnation treatments and carbonization treatments as necessary,
Graphite treatment at 1600-3000 ° C for carbon fiber reinforcement
This is a method for manufacturing a jig material for manufacturing a glass container in which a high-temperature glass container comes into direct contact with a carbon material and is processed into a predetermined shape.

[0006] The short fibers of carbon fibers for reinforcement used in the present invention refer to chops of short fibers or continuous fibers not based on continuous spinning, and may be any of polyacrylonitrile, rayon, and pitch. It may be either carbonaceous or graphite.

The pitch powder serving as a matrix is melted by heating, and has a function as a binder for binding and shaping carbon fibers at the time of molding.
Oil or tar pitch may be used,
Those having a high residual carbon ratio after firing are desirable. In that sense, a pitch having a high softening point, preferably a softening point of 150 to 350
C., more preferably 200 to 300.degree. C. tar pitch is advantageous. On the other hand, if the particle size of the pitch powder is too large, the pitch does not sufficiently enter between the carbon fibers, so that a high strength C /
In order to obtain a C composite, the particle size is desirably 100 μm or less.

[0008] The ratio of short fibers of carbon fiber and pitch powder is
When a C / C composite is used, the carbon fiber content is 5
It is desirably about 60% by volume, preferably about 10% to 45% by volume. For the purpose of increasing the residual carbon ratio, carbonaceous powder such as coke and graphite may be added.
Also in this case, the content of the carbon fiber is preferably set in the above range.

The raw material containing carbon fibers and pitch is used as a water-dispersed slurry. As a method for this, a prepreg or the like may be put in advance and then put into water, or both may be put into water separately. And may be dispersed to form a slurry.

[0010] The aqueous dispersion slurry is filtered to form a raw material layer on the surface of the filter medium to prepare a preform. A wire mesh or the like is used as the filter medium, and the surface shape is set in advance so that a preform having a desired shape is obtained. For example, when obtaining a planar shape, a filter medium having a flat surface is used, and when obtaining a cylindrical shape, a cylindrical filter medium is used. Filtration can be carried out by suction filtration or pressure filtration, but a continuous pressure filtration method is excellent for improving uniformity and precision of shape. According to this method, a layer of the raw material is gradually formed on the surface of the filter medium according to the flow of the slurry, but if there is a difference in the thickness of the layer of the raw material, a difference occurs in the flow of the slurry, and as a result, a uniform The thickness of the layer.

When a predetermined thickness is obtained, the filtration is stopped and the preform is taken out. The obtained preformed body is subjected to processing such as cutting and bending, if necessary, and then compression molded. Examples of the compression molding method include a hot press method performed under heating, an autoclave molding method, a rubber press method, and a vacuum molding method.

[0012] The obtained compact is heated to 800 ° C or higher, preferably 1000 ° C in a non-oxidizing atmosphere such as nitrogen or argon.
Carbonization and calcination at a temperature of not less than 1500 ° C. to obtain a C / C composite intermediate. In this case, if the rate of temperature rise during carbonization is too fast, shrinkage due to thermal decomposition of the pitch and gas generation become severe, and large cracks are likely to occur. Therefore, the heating rate is usually 100 ° C./hr or less, preferably 20 ° C./hr.
hr or less is desirable. Further, at this time, carbonized and baked under pressure for the purpose of suppressing the swelling of the pitch, or as described in JP-A-62-241871 according to the present inventors, the molded body is heated at a high temperature. Alternatively, carbonization and firing may be performed in a state where the fixing is performed using a fixing material that does not deform. The C / C composite intermediate thus obtained is impregnated with a pitch or a thermosetting liquid resin, if necessary, in order to improve the oxidation resistance and mechanical strength of the final product, and is then fired again. Operation and / or chemical vapor deposition (CV)
D process).

In the impregnation treatment, the C / C composite intermediate is placed in a closed container, the pressure in the container is reduced to several tens of mmHg or less, and the gas remaining in the container is expelled. A thermosetting liquid resin as a raw material is poured, and the inside of the container is further filled with 5 to 100 kgf / cm.
At a pressure of 2, impregnate the C / C composite intermediate with the material. Usually, as the impregnating material used here, a liquid thermosetting resin such as a pitch or phenol resin or a furan resin is used. In this case, the substance may be heated in order to adjust the viscosity. CVD
In the treatment, the C / C composite intermediate is placed in a furnace and
The mixture is heated to 000 to 1500 ° C., and a hydrocarbon gas such as methane or propane is diluted with nitrogen, argon or the like, and introduced under reduced pressure to crack and carbonize, thereby depositing pyrolytic carbon on the carbon fiber surface.

Further, the intermediate of the C / C composite, or an operation of impregnating the intermediate and refiring, and / or
Alternatively, the material subjected to the chemical vapor deposition treatment may be subjected to a graphitization treatment as necessary in order to improve the oxidation resistance and thermal conductivity of the final product. The graphitization treatment is usually performed in a non-oxidizing atmosphere such as argon at 1600 to 3000C, preferably 2000 to 3000C.

The C / C composite thus obtained has not only a low carbon fiber orientation and the like, and excellent uniformity, but also short fibers of carbon fibers are completely opened in water,
Since they are three-dimensionally entangled, the interlayer shear strength is high and delamination hardly occurs during processing. In addition, since pitch, which is a graphitizable material, is used as a matrix material, when used as a jig material for glass production,
It is characterized by high oxidation resistance and abrasion resistance.

The C / C composite is then processed into a predetermined shape to obtain a glass container manufacturing jig. The jig material for manufacturing a glass container referred to in the present invention is a dead plate such as a machine dead plate, a takeout tong, a pusher pad, a wear transfer pad, a pad of a stacker bar, and the like, and a member to which a high-temperature glass container directly contacts. Can be applied to Processing into a predetermined shape means that dead plates are cut to a predetermined size, grooves are formed parallel to the transport direction to improve the sliding of the glass container, and air holes for cooling are used. And for tongs,
In order to pinch and hold the neck of the glass container, cutting such as to have a semicircular curved portion that fits the contour of the neck, etc.For pads, cutting and cutting to a predetermined size Drilling holes for screwing or riveting, and cutting the surface in contact with the glass container into a triangle or the like according to the shape of the container. In particular,
Dead plates, which are members that require precise processing,
The application to tongs is advantageous in fully exhibiting the characteristics of this material.

[0017]

EXAMPLE 1 A chop of polyacrylonitrile-based carbon fiber having a fiber length of 10 mm and a pitch fine powder having a softening point of 250 ° C. were dispersed in water at a ratio of 1: 2 (weight ratio), and a 30 × 30 cm flat powder was dispersed. The slurry was pumped into a preforming tank in which a filter medium was set, and filtered. When the thickness became about 5 cm, the filtration was stopped to obtain a preform. This plate-shaped preform is 550
The temperature was raised to 100 ° C. at a rate of 100 ° C./hr, hot pressed, and then carbonized at 1000 ° C. to obtain a C / C composite intermediate (primary carbonized product). The carbon fiber content of this primary carbonized product was 55% by volume. Next, this C / C
200 ° C, 10kg pressure for composite intermediate
/ Cm ² , impregnated with the impregnated pitch, heated to 1000 ° C. at a rate of 10 ° C./hr in a nitrogen atmosphere, and then gradually cooled to obtain a C / C composite intermediate (2). The following carbonized product was obtained. Further, this intermediate was repeatedly impregnated with the pitch and carbonized three times in the same manner as described above. Thereafter, the temperature was raised to 2000 ° C. in an argon atmosphere, maintained for 1 hour, and graphitized to obtain a carbon fiber reinforced carbon material.

From this carbon fiber reinforced carbon material, a width of 3 m
m, depth 2mm, length 280mm groove 6mm in the center
Eleven provided at intervals, width 195 mm x length 280 mm x
An 8 mm thick dead plate was cut out. Similarly, a flat plate having a width of 70 mm × length 70 mm × thickness 6.35 mm is cut out, a hole having a diameter of 30 mm is formed in the center, and cut in half so as to pass through the center line of the opening. I got Processing is performed using a carbide tool, and the resulting dead plate and tongs are free from chipping and scratches at the ends,
It was clean.

Comparative Example 1 Eight-sheet satin-woven polyacrylonitrile-based carbon fiber cloth (3
000 filament) to phenolic resin (AV light)
RM-3000A) was impregnated with a 30% by weight aqueous solution and dried to obtain a prepreg. The prepreg was laminated on a mold and press-molded at a temperature of 150 ° C. under a pressure of 50 kg / cm 2 to obtain a molded body. Next, the molded body was heated to 1000 ° C. at a rate of 10 ° C./hr in a nitrogen atmosphere, and then gradually cooled to obtain a C / C composite intermediate (primary carbonized product). The carbon fiber content of this primary carbonized product was 55% by volume. Next, pitch impregnation and carbonization treatment were repeated four times in the same manner as in Example 1 for the C / C composite intermediate, and subsequently the temperature was raised to 2000 ° C. in an argon atmosphere.
It was graphitized for 1 hour to obtain a carbon fiber reinforced carbon material.
From this carbon fiber reinforced carbon material, in the same manner as in Example 1,
Cut out tongs.

Comparative Example 2 A tongue was cut out of a high-density graphite material currently used for manufacturing glass containers in the same manner as in Example 1 for comparison.

The carbon fiber reinforced carbon materials or the high-density graphite materials of the examples and the comparative examples were air-flowed (500 cc /
min) at 400 ° C. for 24 hours to carry out an oxidation test and a three-point bending test at room temperature. The tongs obtained in the examples and comparative examples were evaluated for performance under the following conditions using a wear tester. The amount of wear at this time was evaluated by rubbing the surface of the tongue with a glass round bar and determining the depth of the cut groove. [Test conditions] Load: 1.5 kg Counterpart material: glass round bar Sliding width: 20 mm Number of sliding times: 1000
Rotation sliding speed: 21 mm / sec Table 1 shows the test results.

[0022]

[Table 1]

As described above, the carbon fiber reinforced carbon material produced by the present method has a higher strength than a current high-density graphite material as a jig material for producing a glass container, and has excellent wear resistance. Further, it can be seen that the oxidation resistance is higher and the abrasion resistance is superior to that of the carbon fiber reinforced carbon material in which the conventional cloth is laminated.

[0024]

According to the method of the present invention, it is possible to produce a jig material for producing a glass container having good workability, excellent oxidation resistance and abrasion resistance.

──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int. Cl. ⁷ , DB name) C04B 35/52 C03B 35/00

Claims (2)

(57) [Claims] An aqueous slurry of a raw material containing short fibers of carbon fiber and pitch powder is filtered to form a layer of the raw material on a surface of a filter medium having a predetermined surface shape, thereby forming a preform. After compression molding of the compact, carbonization treatment, 1
Graphitized carbon fiber reinforced carbon at 600-3000 ° C
A method for manufacturing a jig material for manufacturing a glass container, wherein a high-temperature glass container is directly in contact with the material, the material being processed into a predetermined shape. 2. It contains short fibers of carbon fiber and pitch powder.
Filter the aqueous dispersion slurry of the raw material to
A layer of raw material is formed on the surface of the
After compression molding of this preform,
Obtain the primary carbonized product, impregnate the primary carbonized product one or more times,
Carbonized, then graphitized at 1600-3000 ° C
Into a carbon fiber reinforced carbon material
High temperature glass container is directly contacted
Of manufacturing jig materials for manufacturing glass containers.