JPH11217204A - Production of vitreous carbonaceous member - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a multilayer, thick-walled vitreous carbonaceous member by mutually jointing the respective joint surfaces of a plurality of vitreous carbonaceous members while immersing the member is a liquid thermosetting resin through curing the resin followed by carbonizing the members under heating to reduce developing texture defects such as pores and cracks at the joints. SOLUTION: This multilayer, thick-walled vitreous carbonaceous member is obtained by the following process: the respective joint surface 1S of a plurality of vitreous carbonaceous members are immersed in a liquid thermosetting resin 2 or a solution thereof held in a glass vessel 3 so as to afford such a state that the resin is filled between the joint surfaces 1S; subsequently, the inside of the glass vessel 3 is pref. deaerated under reduced pressure via an evacuation pipe 4; the joint surfaces 1S are directly jointed to each other through curing the resin to prevent generation of air bubbles at the joints; in this case, it is preferable that the joint surfaces 1S are mutually pressed by the aid of a weight 5 or the like; after curing the resin at <=250 deg.C or so, the members are heated at about >=400 deg.C in a nonoxidative atmosphere and carbonized, followed by, as necessary, treatment under heating up to 3,000 deg.C or so (graphitization).

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of manufacturing a large glassy carbon member by joining members made of glassy carbon, and more particularly to a method for cleaning precision parts such as semiconductors and liquid crystals in a semiconductor temperature control device. The present invention relates to a method for producing a member made of glassy carbon suitable for a heat transfer plate for heating a cleaning liquid used in the method.

[0002]

2. Description of the Related Art Glassy carbon has a very dense glassy continuous structure, and has been used in the field of semiconductors, taking advantage of its features such as a small amount of fine particles falling off the structure and being impermeable. Came. For example, it is used for a cleaning liquid heating heat transfer plate used for cleaning precision components in a semiconductor temperature controller. As shown in FIG. 2, the temperature control device for semiconductor includes a heat transfer plate 1 provided at a lower portion of a container 10.
1, a heat source 12 for transmitting heat to the heat transfer plate, a cleaning liquid inlet 13, and a cleaning liquid outlet 14. Fifteen
Is a cleaning liquid.

[0003] Vitreous carbon is obtained by heating and curing thermosetting resin.
Although it is obtained by carbonization, pores and cracks are likely to occur in the structure due to the effects of volatile components from the resin, etc., so flat products with a thickness of up to about 5 mm are mainly used alone, and thick products are required. In many cases, products with special shapes rely on methods such as joining.

Heretofore, for joining glassy carbon members, a method of applying an adhesive such as a thermosetting resin to the joint, heating and curing, and then carbonizing at a high temperature as necessary has been adopted. However, when the bonding surface is a surface of about φ10 cm or more, there is a problem that air bubbles are easily entangled in the bonding portion and defects such as pores and cracks are easily generated in the structure of the bonding portion.

[0005]

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a large glassy carbon member having few structural defects such as pores and cracks at a joint.

[0006]

In order to achieve the above object, the present invention relates to a method for joining a plurality of glassy carbon members, wherein the joining surface is made of a liquid thermosetting resin or a thermosetting resin solution. In the state of being immersed in the steel sheet, it is characterized in that it is taken out after hardening and joining, and then carbonized by heating.

According to the present invention, in joining a plurality of glassy carbon members, the joint surface is evacuated under reduced pressure while immersed in a liquid thermosetting resin or a thermosetting resin solution,
It is characterized in that it is hardened and joined in the liquid as it is, then taken out and carbonized by heating.

[0008]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A method for manufacturing a glassy carbon member according to the present invention will be described below with reference to FIG. The glassy carbon member 1 used in the present invention is generally formed by casting a thermosetting resin such as a phenol-based or furan-based resin and heating and curing at 250 ° C. or lower, and then about 400 to 3000 ° C. in a non-oxidizing atmosphere. It is obtained by heating and carbonizing up to

The thermosetting resin 2 used for bonding is
Any material that turns into glassy carbon after carbonization can be used, but it must be in a liquid state or a powdery state dissolved in a solvent and made into a liquid state. In addition, the same as the base material resin, or phenol resin and furan resin or similar composition (phenol-based for phenol-based, furan-based for furan-based)
Is more preferable because it is easily assimilated with the base material.

[0010] In order to perform the hardening bonding in the liquid, the bonding surfaces 1S, 1S of the pair of glassy carbon members are immersed in a liquid thermosetting resin 2 or a thermosetting resin solution placed in a glass container 3, and Between the joining surfaces 1S, 1S. Since the effect of avoiding pores and cracks is high, it is preferable that the inside of the glass container 3 is degassed under reduced pressure by a vacuum pump or the like (not shown) via the exhaust pipe 4.

Before degassing under reduced pressure, a pair of joint surfaces 1
The thickness of the resin existing between S and 1S (the gap between the joining surfaces 1S and 1S) is not particularly limited, but is preferably 1 μm to 5 μm.
The thickness is preferably set to 00 μm. If a pair of glassy carbon members are brought into close contact with each other before they are immersed in the liquid, it is difficult to fill the gap with the resin, so that a sufficient effect cannot be obtained.

As for the degree of vacuum at the time of degassing under reduced pressure, degassing is promoted if the pressure is lower than the atmospheric pressure (） 760 Torr), but is preferably about 100 Torr or less from the viewpoint of degassing efficiency, and is preferably 10 Torr or less. More preferred.

Degassing under reduced pressure while immersed in a thermosetting resin solution and curing and bonding in the liquid as it is prevents generation of bubbles on the bonding surface. In addition, when the viscosity of the thermosetting resin liquid is low, bubbles are not generated even if the pressure is not reduced. In such a condition, the decompression and deaeration can be omitted.

At the time of hardening bonding in a liquid, it is preferable to press the bonding surface 1S with a weight 5 or the like. The heating conditions during curing and carbonization may be in accordance with the general production conditions for glassy carbon. Usually, after curing at 250 ° C. or lower, under a non-oxidizing atmosphere (such as under vacuum or a nitrogen gas atmosphere). Heat to 400 ° C. or more to carbonize, and perform heat treatment (graphitization) up to about 3000 ° C. as necessary.

Needless to say, three or more glassy carbon members can be joined to form a multilayer glassy carbon member by the above method.

According to the conventional method, as a good glassy carbon having almost no bubbles, only a glass having a thickness of at most about 5 mm can be obtained. However, according to the method of the present invention, no bubbles are generated, so Thick glassy carbon can be obtained.

[0017]

Embodiments of the present invention will be described below. The glassy carbon member 1 has a thickness of 5 mm and a joint surface of 100 ×
100mm glassy carbon flat plate (PXG manufactured by Hitachi Chemical Co., Ltd.)
Liquid phenolic resin (VP manufactured by Hitachi Chemical Co., Ltd.)
-13N), put the weight 5 on the stacked flat plate,
It was pressed at a pressure of 30 g / cm ² . At this time, the distance between the joining surfaces between the two flat plates was 300 μm. Next, cover the glass container 3 with a vacuum pump to
After reducing the pressure to rr or less and deaeration, the pressure was returned to the atmospheric pressure, and the temperature was raised from room temperature to 80 ° C. at a rate of 1 ° C./h in an electric dryer to perform primary curing.

Next, the cured glassy carbon bonded body is taken out of the glass container, and the surrounding resin cured material is removed. After that, the temperature is raised again to 180 ° C. at a rate of 2 ° C./h in an electric dryer. Warm to complete cure. Next, heating to 1200 ° C. in a non-oxidizing atmosphere to carbonize the joint,
The periphery was machined to obtain a glassy carbon bonded body having a thickness of 10 mm. No pores or cracks were observed on the bonding surface of the glassy carbon bonded body.

(Comparative Example) The above-mentioned phenolic resin was applied to the joining surface of the glassy carbon flat plate 1 in the air with a rubber spatula in the same manner as in the example, and then a weight was put thereon and pressed.
Curing and carbonization were performed under the same temperature raising conditions as in the example to obtain a glassy carbon bonded body.

When the bonded surface of the glassy carbon bonded body obtained by the method of the comparative example was observed with a microscope, pores were observed in some places.

[0021]

According to the method for manufacturing a vitreous carbon member according to the present invention, it is possible to reduce structural defects such as pores and cracks at the joint of vitreous carbon, and to produce a thick vitreous carbon member. can do.

[Brief description of the drawings]

FIG. 1 is an explanatory view showing a method for manufacturing a glassy carbon member in an example of the present invention.

FIG. 2 is a longitudinal sectional view of a general semiconductor temperature controller.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Glassy carbon member, 1S ... Joining surface, 2 ... Liquid thermosetting resin, 3 ... Glass container, 4 ... Exhaust pipe, 5 ... Weight

Claims (2)

[Claims] When joining a plurality of vitreous carbon members, the joining surfaces are immersed in a liquid thermosetting resin or a thermosetting resin solution, and after being cured and joined, taken out and heated and carbonized. A method for producing a glassy carbon member, comprising: 2. A method for joining a plurality of glassy carbon members, wherein the joining surfaces are immersed in a liquid thermosetting resin or a thermosetting resin solution, degassed under reduced pressure, and then cured and joined in the liquid. A method for producing a glassy carbon member, wherein the member is taken out and heated and carbonized.