JP2010173873A - Ceramic joined body and supporting member using the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a ceramic joined body without disturbing the flow of heated or cooled fluid, and also without leaking the fluid. <P>SOLUTION: The ceramic joined body 1 is obtained by joining a substrate 2 provided with a flow passage 5 flowing fluid which is formed on the upper face so as to be a groove shape, an inner cover 3 having a shape matching to the flow passage 5 and covering the flow passage 5, and an outer cover 4 covering the upper faces of the inner cover 3 and the substrate 2 which are made of the same ceramic, respectively by a joining layer 7 made of the material same as that of the ceramic, and is provided with an entrance 6 for fluid passing through from the flow passage 5 to the substrate 2 or the outer cover 4. Even if fluid heated to high temperature or fluid subjected to cooling is passed through from the entrance 6 of fluid to the flow passage 5, since the characteristics of the substrate 2, the inner cover 3, the outer cover 4 and the joining layer 7 are the same, and the production of a difference in thermal expansion and shrinkage is reduced, failures such as cracks in the joining layer 7 are made hard to be generated. Further, since the flowing of a joining agent into the flow passage is reduced, fluid can be satisfactorily made to flow through the flow passage over a long period. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a ceramic joined body in which a flow path for passing a fluid such as highly corrosive gas or heated or cooled liquid is formed by joining ceramics, and a support member using the ceramic joined body.

  Conventionally, ceramics have been used for members that pass fluids such as highly corrosive gases and heated or cooled liquids. Since this ceramic has excellent mechanical properties, it is difficult to process, and it is not easy to form a flow channel for flowing a fluid in a ceramic substrate, so a groove made of ceramic was formed. A ceramic joined body in which a flow path is formed by joining a base material and a base material made of another ceramic and covering a groove is used.

  4A and 4B show a conventional ceramic joined body, in which FIG. 4A is a plan view and FIG. 4B is a cross-sectional view taken along line X-X ′ in FIG.

  As shown in FIG. 4, a conventional ceramic joined body 10 includes a first ceramic substrate 12 having a groove-shaped flow path 15 and a second ceramic substrate 14 having a fluid inlet / outlet 16 at the center. However, it joins by the joining layer 17 by apply | coating resin-type or glass-type joining agents to a mutual joining surface, and heat-processing (for example, refer patent document 1).

Patent Document 1 discloses a method for joining a first joint surface of a first ceramic base material and a second joint surface of a second ceramic base material, the first joint surface before joining. And the center line average surface roughness Ra of the second bonding surface is 1.0 μm or less, and the flatness of the first bonding surface and the second bonding surface before bonding is 50 μm or less, The contact area when contacting the second bonding surface is 200 cm ² or more, and the first ceramic substrate and the second ceramic substrate are applied while applying pressure in a direction substantially perpendicular to the first bonding surface. There has been proposed a method for joining ceramic substrates, in which a ceramic substrate is heated and re-sintered to obtain a joined body of a first ceramic substrate and a second ceramic substrate. Further, it is described that a heat treatment is performed after interposing a solution containing an effective sintering aid as a bonding agent between the first bonding surface and the second bonding surface, as an example. In the case where the ceramic substrate is made of aluminum nitride or silicon nitride, it is described that it is preferable to use one or more joining aids selected from the group consisting of yttria compounds, ytterbium compounds and alkaline earth element compounds. ing.

Japanese Patent Laid-Open No. 2002-47071

  However, in the conventional ceramic joined body and the ceramic joined body having the structure described in Patent Document 1, the bonding agent used for joining melts during application and heat treatment and flows into the groove and solidifies, so that the inner wall of the flow path is solidified. There is a problem in that solidified bonding agent is present to prevent a good flow of fluid.

  In addition, when the bonding agent is resin-based, if the temperature of the heated fluid exceeds the melting temperature of the resin-based bonding agent, the resin-based adhesive melts and the fluid leaks from the flow path. .

  Further, when the ceramic base material and the bonding layer are of different materials, the thermal expansion and contraction of the ceramic base material and the bonding layer differ depending on the temperature of the fluid flowing through the flow path, and the bonding layer gradually deteriorates, There was a problem that fluid leaked from the flow path.

  The present invention has been devised to solve the above problem, and the ceramic joined body in which the flow of the fluid heated or cooled in the flow path is not hindered and the fluid does not leak from the flow path. And it aims at providing a supporting member using the same.

  The ceramic joined body of the present invention, each made of the same ceramic, a base provided with a flow path for flowing a fluid formed in a groove shape on the upper surface, an inner lid that covers the flow path in a shape that matches the flow path, The inner lid and an outer lid that covers the upper surface of the base are joined by a joining layer that is the same as the ceramic, and an inlet / outlet for the fluid that passes through the base or the outer lid from the flow path is provided. It is characterized by this.

  Further, the ceramic joined body of the present invention is characterized in that, in the above configuration, the inner lid has a width smaller than a width of the opening of the flow path and at least a part thereof is disposed in the flow path. It is.

  Moreover, the ceramic joined body of the present invention is characterized in that, in any one of the above-described structures, the inner lid is fitted into a step provided at an edge of the opening of the flow path.

  Moreover, the ceramic joined body of the present invention is characterized in that, in the above configuration, the side surface of the inner lid and the step are joined.

  Moreover, the ceramic joined body of the present invention is characterized in that, in any one of the above structures, the base body, the inner lid, and the outer lid are made of a high-purity alumina sintered body.

  The method for producing a ceramic joined body according to the present invention is a method for producing a ceramic joined body having the above-described configuration, and uses a secondary raw material that is granulated by spray drying a slurry in which a ceramic raw material, a binder and a solvent are mixed. A step of obtaining a molded body of the base body, the inner lid and the outer lid; a step of forming a groove-like channel on the upper surface of the molded body of the base body; and at least one of the molded body of the base body and the molded body of the outer lid. On the other hand, a step of forming an inlet / outlet through which the fluid passes through the flow path, and a bonding agent made of a slurry in which the ceramic raw material, a binder and a solvent are mixed, are used as at least one of the molded body of the base and the molded body of the inner lid. It is applied to the joint, and the molded body of the base body and the molded body of the inner lid are integrated to dry the bonding agent, thereby obtaining a first bonded molded body in which the base body and the inner lid are integrated. And the process The bonding agent is applied to at least one of the joint surfaces of the joint molded body and the outer lid molded body, and the first joint molded body and the outer lid molded body are placed inside the molded body of the inner lid. Arranging and integrating to dry the bonding agent to obtain a second bonded molded body in which the base body, the inner lid and the outer lid are integrated; and firing the second bonded molded body. And a process.

  In the method for manufacturing a ceramic joined body according to the present invention, in the above configuration, a step is formed at an edge of an opening of a flow path formed in the molded body of the base body, and the molded body of the inner lid is fitted into the step. The method further comprises the step of putting the bonding agent into a gap between the step and the side surface of the molded body of the inner lid, and drying the bonding agent to obtain the first bonded molded body.

  The support member according to the present invention is characterized in that the ceramic joined body having any one of the above-described structures is used for supporting a placement object.

  According to the ceramic joined body of the present invention, each of the same ceramics, the base having a flow path for flowing the fluid formed in a groove shape on the upper surface, an inner lid that covers the flow path in a shape that matches the flow path, The inner lid and the outer lid that covers the upper surface of the base are joined by a bonding layer of the same quality as the ceramic, and the fluid inlet / outlet is provided from the flow path through the base or the outer lid. Even if a fluid heated to high temperature or a cooled fluid is passed through the flow path, the characteristics of the base, inner lid, outer lid, and bonding layer are the same, and there is little difference in thermal expansion and contraction. It is possible to reduce the occurrence of defects such as cracks due to deterioration of the bonding layer. In addition, since the bonding agent is less likely to flow into the flow channel than in the past, it is possible to prevent foreign matter from adhering to the inner wall of the flow channel, and the fluid can flow well through the flow channel over a long period of time.

  Further, according to the ceramic joined body of the present invention, when the width of the inner lid is smaller than the width of the opening of the flow path and at least a part of the inner lid is disposed in the flow path, Since the flow path is sealed by the bonding layer bonding the lid and the bonding layer bonding the upper surface of the base body and the inner lid and the outer lid, the fluid is less likely to leak from the flow path. It is possible to obtain a ceramic joined body excellent in sealing performance against leakage from the flow path.

  Further, according to the ceramic joined body of the present invention, when the inner lid is fitted in the step provided at the edge of the opening of the flow path, the lower surface and the side surface of the inner lid serve as a joined portion, and the base and the inner lid The bonding strength can be increased and the sealing performance against leakage from the fluid flow path can be further improved.

  Moreover, according to the ceramic joined body of the present invention, when the side surface of the inner lid and the step are joined, it is possible to reliably prevent the flow of the fluid in the flow path into the flow path. Good flow can be ensured.

  Further, according to the ceramic joined body of the present invention, when the base body, the inner lid and the outer lid are made of a high-purity alumina sintered body, the corrosion resistance against the highly corrosive fluid of the base body, the inner lid, the outer lid and the joining layer. Therefore, it can be suitably used for applications such as a semiconductor manufacturing process in which various corrosive fluids are passed through the flow path.

  Further, according to the method for producing a ceramic joined body of the present invention, a molded body of a base body, an inner lid, and an outer lid using a secondary raw material obtained by spray drying and granulating a slurry in which a ceramic raw material, a binder and a solvent are mixed. A step of forming a groove-like channel on the upper surface of the molded body of the substrate, and a step of forming an inlet / outlet through which the fluid flows in at least one of the molded body of the substrate and the molded body of the outer lid And a bonding agent comprising a slurry in which a ceramic raw material, a binder and a solvent are mixed, is applied to at least one joint portion of the base molded body and the inner lid molded body, and the base molded body and the inner lid molded body are integrated. And drying the bonding agent to obtain a first bonded molded body in which the base body and the inner lid are integrated, and a bonding agent on at least one bonding surface of the first bonded molded body and the outer lid molded body Apply the first bonded molded body and the outside A step of obtaining a second bonded molded body in which the base, the inner lid, and the outer lid are integrated, by integrating the molded body of the inner lid with the molded body of the inner lid disposed therein and drying the bonding agent; And a step of firing the bonded molded body of 2 can be obtained such that a ceramic bonded body that can be integrated and sufficiently densified so that the boundary between the bonding layer and the substrate, the inner lid, and the outer lid is not known. .

  Further, according to the method for manufacturing a ceramic joined body of the present invention, a step is formed at the edge of the opening of the flow path formed in the base body, and the step of the inner lid is fitted into the step. When a bonding agent is put into the gap between the side surface of the molded body and the bonding agent is dried to obtain the first bonded molded body, the flow of the bonding agent into the flow path is small and the fluid flow is good. A ceramic joined body having a simple flow path can be obtained.

  According to the support member of the present invention, since the ceramic joined body of the present invention is used for supporting the object to be placed, the flow of the bonding agent into the flow path is small, and the fluid flows well in the flow path. Since it is excellent in the sealing performance against leakage from the fluid, the heated or cooled fluid can be suitably flowed through the flow path, so that the mounted object can be heated or cooled satisfactorily. Moreover, since it has the intensity | strength which can fully bear the weight of a mounted article, it can be used suitably as a supporting member.

An example of embodiment of the ceramic joined body of this invention is shown, (a) is a top view, (b) is sectional drawing in the A-A 'line of (a). The other example of embodiment of the ceramic joined body of this invention is shown, (a) is a top view, (b) is sectional drawing in the B-B 'line | wire of (a). Still another example of the embodiment of the ceramic joined body of the present invention is shown, (a) is a plan view, and (b) is a sectional view taken along line C-C 'of (a). FIG. 5A is a plan view showing a conventional ceramic joined body, and FIG. 5B is a cross-sectional view taken along line X-X ′ in FIG.

  Hereinafter, examples of embodiments of the ceramic joined body of the present invention will be described with reference to the drawings.

  1A and 1B show an example of an embodiment of a ceramic joined body of the present invention, in which FIG. 1A is a plan view and FIG. 1B is a cross-sectional view taken along line A-A ′ of FIG.

  The ceramic joined body 1 of the present invention includes a base 2 having a flow path 5 for flowing a fluid formed in the shape of a groove on the upper surface, each made of the same ceramic, and an inner surface that covers the flow path 5 in a shape that matches the flow path 5. The lid 3 and the outer lid 4 that covers the inner lid 3 and the upper surface of the base body 2 are joined by a joining layer 7 that is the same quality as ceramics, and a fluid inlet / outlet 6 that passes through the base body 2 or the outer lid 4 from the flow path 5 is provided. Is provided. As described above, the base body 2, the inner lid 3 and the outer lid 4 are made of the same ceramics, and are joined by the homogeneous joining layer 7, so that the fluid heated from the fluid inlet / outlet 6 to the flow path 5 at a high temperature. Even if the cooled fluid is passed, the characteristics of the base body 2, the inner lid 3, the outer lid 4 and the bonding layer 7 are the same, and there is little difference in thermal expansion and contraction. As a result, defects such as cracks are less likely to occur.

  Further, as shown in FIG. 1, the channel 5 formed in a groove shape on the base 2 is covered with an inner lid 3 having a shape matching the channel 5, and the upper surface of the inner lid 3 and the base 2 is covered with the outer lid. 4, and the bonding layer 7 is held up to the upper surface of the base 2 so that the bonding layer 7 is not provided inside the flow channel 5. Compared to a ceramic joined body having a structure that is closed only with a lid, the bonding agent is less likely to flow into the flow path 5, and the fluid can flow through the flow path 5 well over a long period of time.

  Here, any fluid can be used as the fluid flowing through the flow path 5 of the ceramic joined body 1 of the present invention as long as it is a heat medium used as various liquids or gases. As the heating heat medium, for example, a liquid such as water, oil, silicon oil, or water vapor can be used. As the cooling heat medium, for example, liquids such as water, acetone, liquid nitrogen, brine (antifreeze), Galden (registered trademark), and gases such as ammonia, chlorofluorocarbon, and carbon dioxide can be used.

  2A and 2B show another example of the embodiment of the ceramic joined body of the present invention. FIG. 2A is a plan view, and FIG. 2B is a sectional view taken along line B-B ′ in FIG.

  Thus, in the ceramic joined body 1 of the present invention, it is preferable that the width of the inner lid 3 is smaller than the width of the opening of the flow path 5 and at least a part of the inner lid 3 is disposed in the flow path 5. Thus, the flow path includes the inner lid 3, the bonding layer 7 that bonds the base 2 and the inner lid 3, and the bonding layer 7 that bonds the upper surface of the base 2 and the inner lid 3 and the outer lid 4. 5 is sealed, the fluid hardly leaks from the inner lid 3 side of the flow path 5, and the ceramic joined body 1 having excellent sealing performance against leakage of the fluid from the flow path 5 can be obtained.

  In the example shown in FIG. 2, the shape of the inner lid 3 is a flat plate. Since such an inner lid 3 has a simpler shape than the inner lid 3 constituting the ceramic joined body 1 of the present invention shown in FIG. 1, it can be easily manufactured. Further, as shown in FIG. In addition, since the upper surface of the base 2 and the upper surface of the inner lid 3 are flush with each other, a process for forming a recess corresponding to the inner lid 3 protruding from the upper surface of the base 2 is performed on the outer lid. Since it is not necessary to apply to 4, processing cost can be reduced. Further, since the upper surface of the substrate 2 and the upper surface of the inner lid 3 are flush with each other, it is easy to apply the bonding agent, and the bonding layer 7 having a uniform thickness is formed between the substrate 2 and the outer lid 7. Therefore, stress concentration due to the load applied when the ceramic joined body 1 of the present invention is used as a support member for the object to be placed is less likely to occur. Further, since the thickness of the bonding layer 7 can be reduced, the bonding strength is increased, which is preferable.

  3A and 3B show still another example of the embodiment of the ceramic joined body of the present invention. FIG. 3A is a plan view, and FIG. 3B is a cross-sectional view taken along the line CC ′ of FIG. .

  Thus, in the ceramic joined body 1 of the present invention, it is preferable that the inner lid 3 is fitted in the step 8 provided at the edge of the opening of the flow path 5 formed in the shape of a groove on the upper surface of the base 2. In particular, when the contact portion between the step 8 and the inner lid 3 is processed to be flat, the upper surface of the base 2 and the inner lid 3 are more than when the inner lid 3 is disposed on the inclined surface as in the example shown in FIG. It is easy to make the upper surface of the bonding surface flush with each other, it is easy to apply the bonding agent, and the bonding layer 7 having a uniform thickness can be formed between the base 2 and the outer lid 7.

  In the ceramic joined body 1 of the present invention, the side surface of the inner lid 2 and the step 8 provided at the edge of the opening of the flow path 5 are preferably joined. Thereby, since the bonding layer 7 does not exist on the lower surface of the inner lid 3 as in the ceramic bonded body 1 of the present invention shown in FIG. 1B, the flow into the bonding agent into the flow path 5 is surely prevented. And a good flow of fluid can be ensured.

  In the ceramic joined body 1 of the present invention, the base 2, the inner lid 3 and the outer lid 4 are preferably made of a high-purity alumina sintered body. As the base 2, the inner lid 3 and the outer lid 4 each made of the same ceramic, it is possible to apply oxide ceramics such as alumina and zirconia, and non-oxide ceramics such as silicon nitride and silicon carbide. In particular, by using a high-purity alumina sintered body having a purity of 95% or more, it is possible to improve the corrosion resistance of the substrate 2, the inner lid 3, the outer lid 4 and the bonding layer 7 against highly corrosive fluids. Therefore, it can be suitably used for applications such as a semiconductor manufacturing process in which various fluids having corrosive properties are passed through the flow path 5.

  Next, the manufacturing method of the ceramic joined body 1 of this invention is demonstrated.

  First, the process of obtaining the molded body of the base body 2, the inner lid 3 and the outer lid 4 will be described. Prepare a ceramic raw material with a purity of 90% or more and an average particle size of about 1 μm, add a predetermined amount of sintering aid, binder, solvent, dispersant, etc. to this and mix the slurry, then spray granulation method (spray Spray dried by a dry method) and granulated to obtain a secondary material. As ceramic materials used at this time, oxide ceramics such as alumina and zirconia, and non-oxide ceramics such as silicon nitride and silicon carbide can be applied. When used for the purpose of passing through, it is preferable to use a high-purity alumina ceramic raw material having a purity of 95% or more and an average particle diameter of 1 μm or less. Thereby, it can be set as the ceramic joined body 1 excellent in corrosion resistance. Next, the spray-dried and granulated secondary raw material is put into a rubber mold having a predetermined shape and molded by a hydrostatic press molding method (rubber press method). The base 2, the inner lid 3, and the outer lid 4 are cut into a molded body.

  Moreover, about the molded object of the base | substrate 2, the groove-shaped flow path 5 is formed in one main surface (upper surface). Then, an inlet / outlet port 6 through which the fluid flows is formed in at least one of the molded body of the base 2 and the molded body of the outer lid 4. Here, the entrance / exit 6 through which the fluid flows is formed in at least one of the molded body of the base 2 and the molded body of the outer lid 4 according to the use of the ceramic joined body 1. This is because it may be provided on the base 2 and the outer lid 4, or may be provided only on the base 2 or only on the outer lid 4. For example, if the fluid is introduced from the substrate 2 side and is discharged from the substrate 2 side through the flow path 5, at least two inlets / outlets 6 may be provided only in the molded body of the substrate 2, and the fluid is introduced from the outer lid 4 side. If it goes out from the outer lid 4 side through the path 5, at least two entrances 6 may be provided only in the molded body of the outer lid 4. If the fluid inlet side and the outlet side are on different sides of the base 2 and the outer lid 4, the inlet / outlet 6 may be provided in each of the molded body of the base 2 and the molded body of the outer lid 4. Furthermore, if the inner lid 3 has a size that covers all of the flow path 5, the inner lid 3 at a position that overlaps with the inlet / outlet 6 formed in the molded body of the base body 2 or the molded body of the outer lid 4 when joined is also fluid. The entrance / exit 6 may be provided. Further, if the molded body of the inner lid 3 protrudes from the upper surface of the molded body of the base body 2 when the molded body of the base body 2 and the molded body of the inner lid 3 are joined together, What is necessary is just to give the cutting process which forms the recessed part corresponding to the part which the molded object of the lid | cover 3 protrudes.

  Next, the process of joining the molded body of the base body 2, the inner lid 3 and the outer lid 4 will be described. First, the molded body of the base 2 and the molded body of the inner lid 3 are joined. As a bonding agent used for bonding, a predetermined amount of a ceramic raw material, a sintering aid, a binder, a dispersant, and a solvent used for manufacturing the molded body of the base body 2, the inner lid 3 and the outer lid 4 are weighed and mixed. A bonding agent is used. Then, this bonding agent is applied to at least one bonded portion of the molded body of the base body 2 and the molded body of the inner lid 3, and the molded body of the base body 2 and the molded body of the inner lid 3 are integrated to dry the bonding agent. Thus, a first bonded molded body in which the base 2 and the inner lid 3 are integrated is obtained.

  Next, a bonding agent is applied to at least one joint surface of the first bonded molded body and the molded body of the outer lid 4, and the first bonded molded body and the molded body of the outer lid 4 are molded into the molded body of the inner lid 3. Are integrated and dried to obtain a second bonded molded body in which the base body 2, the inner lid 3 and the outer lid 4 are integrated. Thereafter, the second bonded molded body is fired in an air atmosphere at a temperature of 1500 ° C. or higher and 1700 ° C. or lower, so that the overall porosity is 1% or lower, and the bonding layer 7 and the substrate formed by baking the bonding agent 2, it is possible to obtain the ceramic joined body 1 of the present invention which is integrated and sufficiently densified so that the boundary between the inner lid 3 and the outer lid 4 is not known. In addition, about the ceramic joined body 1 after baking, you may grind as needed.

At this time, the powder filling rate of the bonding agent is preferably 20% or more and 50% or less. If the powder filling rate of the bonding agent is within this range, the viscosity can be easily applied to the bonding surfaces of the molded bodies of the base body 2, the inner lid 3 and the outer lid 4, and the bonding agent applied to the bonding surfaces. Since the ceramic particles necessary for densification are sufficiently present therein, the boundary between the bonding layer 7 and the substrate 2, the inner lid 3, and the outer lid 4 can be obtained by drying and baking the bonding agent. It can be integrated so as not to be understood, and can be sufficiently densified. Further, when the bonding agent is applied to integrate the molded body of the base body 2 and the molded body of the inner lid 3, or the first bonded molded body and the molded body of the outer lid 4 are integrated into the molded body of the inner lid 3. When placing and integrating, the load may be applied so that a pressure of 20 kg / cm ² or more is applied to the joint. The powder filling rate of the bonding agent is calculated by dividing the volume of the ceramic raw material powder used for the bonding agent by the volume of the bonding agent and multiplying this value by 100.

  Moreover, as a manufacturing method of the ceramic joined body 1 of the present invention, when the flow path 5 is formed by cutting the molded body of the base body 2, the molded body of the inner lid 3 is formed at the edge of the opening of the flow path 5. A step 8 having a size that can be accommodated is formed, and a molded body of the inner lid 3 is fitted into the step 8, and a bonding agent is put between the step 8 and the side surface of the molded body of the inner lid 3. It is also possible to obtain a first bonded molded body in which the base body 2 and the inner lid 3 are integrated by integrating the molded body of the inner lid 3 and drying the bonding agent.

  In particular, it is preferable that the molded body of the inner lid 3 does not protrude from the upper surface of the molded body of the base body 2 which becomes a joint surface with the molded body of the outer lid 4 and is flattened. Thereby, it becomes easy to apply the bonding agent uniformly when applying the bonding agent to the first bonded molded body, and the second bonded molded body is better integrated with the molded body of the outer lid 4. By firing this bonded molded body, the ceramic bonded body 1 bonded more firmly can be obtained.

  And by making the base | substrate 2 and the outer cover 4 which comprise the ceramic joined body 1 of this invention into plate shape, it can be made suitable for the supporting member used for support of a mounted article. According to this support member, the main body of the base body 2 or the outer lid 4 is used as an upper surface to support the object to be placed, and the heated or cooled fluid is allowed to flow through the internal flow path 5, whereby the ceramic joined body 1 of the present invention. The mounted object can be stably heated or cooled via a certain support member.

  Examples of the ceramic joined body 1 of the present invention are shown below.

  The ceramic joined body 1 of the present invention shown in FIG. 1 is manufactured, and after joining, a fluid heated to 100 to 200 ° C. for a long time is passed through the flow path 5 of the ceramic joined body 1 to leak the fluid from the joined portion. A test was conducted to confirm whether there was any.

  First, alumina having a purity of 99% and an average particle size of 1 μm is prepared as a ceramic raw material, and a slurry obtained by adding a predetermined amount of a sintering aid, a binder, a solvent and a dispersant to the mixture is spray granulated. Spray drying was performed by the method (spray drying method) and granulated to obtain a secondary raw material. The alumina secondary raw material was put into a rubber mold having a predetermined shape and molded by an isostatic press molding method (rubber press method). Thereafter, the molded body was removed from the rubber mold.

  And in order to form the molded object of the base | substrate 2, the cutting process was given to the molded object removed from the rubber mold | type so that it might become a predetermined | prescribed outer shape. Moreover, the cutting process which forms the entrance / exit 6 of the fluid which penetrates from one end of the flow path 5 and the flow path 5 to the other main surface was given to the one main surface (upper surface).

  Next, in order to form a molded body of the outer lid 4, the molded body removed from the rubber mold was cut so as to have a predetermined outer shape. In addition, a cutting process for forming a fluid inlet / outlet 6 at a position corresponding to the other end of the flow path 5 of the molded body of the base 2 was performed.

  Further, in order to form a molded body of the inner lid 3, the molded body removed from the rubber mold was cut so as to have a predetermined outer shape. Further, a cutting process for forming the fluid inlet / outlet 6 was performed at a position overlapping the fluid inlet / outlet 6 formed in the molded body of the outer lid 4.

  Further, regarding the molded body of the outer lid 4, when the molded body of the base body 2 and the molded body of the inner lid 3 are joined to the main surface on the side to be joined to the molded body of the base body 2, the molded body of the inner lid 3. The cutting process which forms the recessed part corresponding to the part which protrudes was performed. These cutting operations were performed using a milling machine or a universal grinder.

  Next, the molded body of the base body 2 and the inner lid 3 was joined. As a bonding agent used for this bonding, a predetermined amount of alumina, which is a ceramic raw material used for manufacturing the molded body of the base body 2, the inner lid 3 and the outer lid 4, and a sintering aid, a binder, a dispersant and a solvent are weighed. Then, a bonding agent made of a slurry having a powder filling rate of 50% was used. Then, a bonding agent is applied to the joint portion of the molded body of the inner lid 3 with a thickness of 100 μm or less, and the molded body of the base body 2 and the molded body of the inner lid 3 are integrated to apply the bonding agent at a temperature of about 100 ° C. By drying, a first bonded molded body in which the base 2 and the inner lid 3 were integrated was obtained.

  Next, a bonding agent is applied to the bonding surface of the first bonded molded body with a thickness of 100 μm or less, and the molded body of the inner lid 3 is placed inside the first bonded molded body and the molded body of the outer lid 4. Then, it was dried and integrated at a temperature of about 100 ° C. to obtain a second bonded molded body in which the base 2, the inner lid 3 and the outer lid 4 were integrated. Thereafter, the second bonded molded body is put into a firing furnace and fired at a temperature of 1600 ° C. in an air atmosphere, the entire porosity is 1% or less, and the bonding layer 7 and the base body obtained by firing the bonding agent 2, the ceramic joined body 1 of the present invention shown in FIG. 1 was obtained, which was integrated and sufficiently densified so that the boundary between the inner lid 3 and the outer lid 4 was not known.

  Further, as a comparative example, a base molded body and an outer lid molded body similar to those of the examples of the present invention are placed in a firing furnace and fired at a temperature of 1600 ° C. in an air atmosphere. A ligature was obtained. And the yttria-type bonding agent was apply | coated to these joining surfaces, the base material and the outer cover were joined, and it heat-processed, and the ceramic joined body of the comparative example was obtained.

  Then, a pipe for passing a fluid through the fluid inlet / outlet 6 of the ceramic joined body 1 of the present invention and the ceramic joined body of the comparative example is connected to the inlet / outlet 6, and silicon oil at 20 ° C., 100 ° C. and 200 ° C. is added every 3 hours. A test for switching to automatic flow control and flowing into the flow path 5 was performed continuously for one week. Thereafter, the colored fluid was cut after passing the ceramic joined body 1 of the present invention and the ceramic joined body of the comparative example through the flow path 5, and each flow path 5 and the bonding layer 7 were confirmed.

  As a result, the ceramic joined body of the comparative example passed a fluid having a temperature difference, so that the joining layer cracked due to the difference in thermal expansion between the base body and the outer lid and the joining layer, and the colored fluid joined from the flow path. It spreads toward the layer. Moreover, it was confirmed that the bonding agent that seems to have melted during the sintering flowed into the flow path. On the other hand, it was confirmed that the ceramic joined body 1 of the present invention hardly spreads from the flow path 5 toward the bonding layer 7 and has high sealing performance of the flow path 5. Further, it was confirmed that there was almost no flow of the bonding agent into the flow path 5 and that the fluid could be suitably flowed.

  A ceramic joined body 1 of the present invention shown in FIGS. 1, 2 and 3 was produced. First, the ceramic joined body 1 of the present invention shown in FIG. 1 was obtained in the same manner as in Example 1.

  Next, the molded body manufactured by the same method as in Example 1 and removed from the rubber mold was cut to have a predetermined outer shape as the molded body of the base body 2 shown in FIG. Moreover, the cutting process which forms the entrance / exit 6 of the fluid which penetrates from the one end of the groove-shaped flow path 5 which has an inclined surface, and the flow path 5 to the other main surface was given to the one main surface (upper surface).

  Next, the molded body removed from the rubber mold was cut so as to have a predetermined outer shape as the molded body of the outer lid 4. In addition, a cutting process for forming a fluid inlet / outlet 6 was performed at a position that is the other end of the flow path 5 of the molded body of the base 2.

  Further, as a molded body of the inner lid 3, the molded body removed from the rubber mold is covered with the flow path 5, is in contact with the inclined surface of the flow path 5 formed in the molded body of the base body 2, and is bonded to the molded body of the base body 2 after bonding. Cutting was applied to a shape having a thickness that is flush with the upper surface. Further, a cutting process for forming the fluid inlet / outlet 6 was performed at a position overlapping the fluid inlet / outlet 6 formed in the molded body of the outer lid 4.

  Further, as the molded body of the base body 2 shown in FIG. 3, the molded body removed from the rubber mold was cut so as to have a predetermined outer shape. Further, a cutting process was performed on one main surface (upper surface) to form a groove-shaped flow path 5 having a step 8 and a fluid inlet / outlet 6 that penetrates from one end of the flow path 5 to the other main surface.

  Next, the molded body removed from the rubber mold was cut so as to have a predetermined outer shape as the molded body of the outer lid 4. In addition, a cutting process for forming a fluid inlet / outlet 6 was performed at a position that is the other end of the flow path 5 of the molded body of the base 2.

  Further, as the molded body of the inner lid 3, when the molded body removed from the rubber mold covers the flow path 5 and is fitted into the step 8 formed on the molded body of the base body 2, the upper surface and the surface of the molded body of the base body 2 are covered. Cutting was applied to a shape having a thickness that can be joined between the side surface of the molded body of the inner lid 3 and the step 8. Further, a cutting process for forming the fluid inlet / outlet 6 was performed at a position overlapping the fluid inlet / outlet 6 formed in the molded body of the outer lid 4.

  About these joining and baking, it carried out by the method similar to Example 1, and obtained the ceramic joined body 1 of this invention shown in FIG. 2 and FIG.

  And the ultrasonic flaw test was done about the ceramic joined body 1 of this invention shown in FIG.1, FIG.2 and FIG.3, and the joining state was confirmed. In the ultrasonic flaw detection test, the ceramic joined body 1 was immersed in a water tank of an ultrasonic flaw detector, an ultrasonic wave was emitted from the probe, and the state of the joint was confirmed from the reflected echo. As a result, the ceramic joined body 1 of the present invention shown in FIG. 2 and FIG. 3 has the upper surface of the base 2 and the inner lid 3 that are flush with each other, so that it is easy to apply the bonding agent. The bonded state was better than that of the ceramic bonded body 1. Further, as a result of the same tests and confirmation as in Example 1, the ceramic joined body 1 of the present invention shown in FIG. 1, FIG. 2 and FIG. 3 has less spread from the flow path 5 toward the joining layer 7. It was confirmed that the sealability of the flow path 5 was high. In addition, it was confirmed that the ceramic joined body 1 of the present invention shown in FIG. 3 has the least amount of the bonding agent flowing into the flow path 5 and can flow the fluid through the flow path 5 more suitably.

  1, 2 and 3, the placed object is supported on the upper surface of the outer lid 4 of the ceramic joined body 1 of the present invention shown in FIG. 1, FIG. 2, and FIG. 3 and the outer lid 4 are integrated so that the boundary between them and the outer lid 4 is not known. The base 2, the inner lid 3 and the outer lid 4 are made of the same ceramics, and these are joined by a homogeneous joining layer 7, thereby Since the thermal expansion and contraction of the base body 2, the inner lid 3 and the outer lid 4 and the bonding layer 7 are the same even when the fluid heated or cooled to 5 is passed, there is little difference in thermal expansion and contraction. It was so small that the layer 7 deteriorated to cause defects such as cracks and the fluid leaked from the flow path 5 so that it could hardly be confirmed. In addition, since the bonding agent hardly flows into the flow path 5 and the heated or cooled fluid can be suitably flowed into the flow path 5, the mounted object can be heated or cooled satisfactorily. Moreover, since it has the intensity | strength which can fully bear the weight of a mounted article, it has confirmed that it could use suitably as a supporting member.

1: Ceramic joined body 2: Substrate 3: Inner lid 4: Outer lid 5: Channel 6: Entrance / exit 7: Joining layer 8: Step

Claims (8)

Each base made of the same ceramics and provided with a channel for flowing a fluid formed in a groove shape on the upper surface, an inner lid covering the channel with a shape matching the channel, the inner lid and the base An outer lid that covers an upper surface is bonded with a bonding layer of the same quality as the ceramic, and a fluid inlet / outlet port that passes through the base body or the outer lid from the flow path is provided. . 2. The ceramic joined body according to claim 1, wherein the inner lid has a width smaller than a width of the opening of the flow path, and at least a part thereof is disposed in the flow path. The ceramic joined body according to claim 1 or 2, wherein the inner lid is fitted into a step provided at an edge of the opening of the flow path. The ceramic joined body according to claim 3, wherein a side surface of the inner lid and the step are joined. The ceramic joined body according to any one of claims 1 to 3, wherein the base body, the inner lid, and the outer lid are made of a high-purity alumina sintered body. A method for producing a ceramic joined body according to claim 1,
Using a secondary raw material granulated by spray drying a slurry in which a ceramic raw material, a binder and a solvent are mixed, and obtaining a molded body of a base, an inner lid and an outer lid;
Forming a groove-like channel on the upper surface of the molded body of the base;
Forming an inlet / outlet for passing the fluid through the flow path in at least one of the molded body of the base and the molded body of the outer lid;
A bonding agent comprising a slurry in which the ceramic raw material, a binder and a solvent are mixed is applied to at least one joint portion of the molded body of the base and the molded body of the inner lid, and the molded body of the base and the molded body of the inner lid. And drying the bonding agent to obtain a first bonded molded body in which the base and the inner lid are integrated;
The bonding agent is applied to at least one joint surface of the first bonded molded body and the outer lid molded body, and the first bonded molded body and the outer lid molded body are combined with the inner lid molded body. A second bonding molded body in which the base, the inner lid, and the outer lid are integrated to obtain a second bonded molded body by integrating and drying the bonding agent;
And a step of firing the second bonded molded body. A step is formed at an edge of the opening of the flow path formed in the molded body of the base body, and the molded body of the inner lid is fitted into the step, and a gap is formed between the step and the side surface of the molded body of the inner lid. The method for producing a ceramic joined body according to claim 6, further comprising a step of adding the bonding agent and drying the bonding agent to obtain the first bonded molded body. 6. A support member, wherein the ceramic joined body according to claim 1 is used for supporting a mounted object.

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