JP2007055853A - Method of manufacturing ceramic composite material - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method of manufacturing a ceramic composite member which is bonded with an adhesive layer being even and free of a bubble, superior in adhesive strength at a high temperature of 200°C or higher, can be suitably used as members for semiconductor/liquid crystal manufacturing apparatuses, especially as a plasma treating apparatus. <P>SOLUTION: A heat-fusing type polyimide film having a thermal decomposition temperature of 300°C or higher and a glass transition temperature of 180°C or higher is sandwiched between a ceramic base material and a yttria ceramic sintered body and pressurized and heated, to prepare a ceramic composite member having tensile strength of an adhesion face at a temperature of 250°C or lower of 0.3 MPa or higher. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for manufacturing a ceramic composite material that can be suitably used in a semiconductor / liquid crystal manufacturing apparatus, in particular, a plasma processing apparatus.

Conventionally, alumina ceramics have been used as plasma-resistant ceramic members used in semiconductor manufacturing equipment.
However, when the alumina ceramic member is exposed to plasma in a corrosive gas atmosphere in the plasma processing step, the corrosion gradually proceeds, the crystal particles constituting the surface fall off, adhere to the semiconductor wafer, It had the subject that performance and reliability were impaired.
Also in the CVD process, since it is exposed to plasma in a fluorine-based gas atmosphere such as fluorine nitride at the time of cleaning after the process, similarly, corrosion resistance against corrosive gas and plasma is required.

  For this reason, yttria ceramics were also used as ceramics with excellent corrosion resistance against corrosive gases. However, yttria ceramics are expensive and inferior in strength to alumina ceramics. It was sometimes difficult.

  In response to this, for example, a member in which a sprayed thin film of plasma-resistant ceramic such as yttria is formed on the surface of a base material made of aluminum, stainless steel, aluminum nitride or the like has been proposed. It was not always easy to form a sprayed coating by force (see Patent Document 1).

In addition, in order to obtain a joined body in which a base material and a plasma-resistant ceramic such as yttria ceramics are combined, for example, mechanical joining such as shrink fitting, brazing, bonding with an adhesive, and the like are firmly joined. A method is being considered.
Among these methods, joining of ceramics using an adhesive is simple and frequently used because an adhesive can be selected according to the use environment.

As the organic adhesive, an epoxy or silicon rubber adhesive is generally used. Since these adhesives have a glass transition temperature of less than 200 ° C., a semiconductor device having a use temperature of 200 ° C. or higher. It was unsuitable for a member for use from the viewpoint of a decrease in adhesive strength and contamination in the chamber.
For this reason, as an adhesive excellent in heat resistance, a polyimide adhesive having a glass transition temperature of about 200 to 400 ° C. has been used (for example, see Patent Document 2).

As an inorganic adhesive, for example, Patent Document 3 discloses an adhesive for ceramics in which an alkali metal silicate containing sodium silicate as a main component and an amorphous silica powder are blended with a ceramic aggregate.
Japanese Patent Laid-Open No. 2004-2101 Japanese Patent Laid-Open No. 9-227852 (paragraph 0004) JP-A-3-192176

  However, the polyimide-based adhesive is in a liquid state, and when applied, like other organic adhesives, bubbles are easily generated in the adhesive layer, and it is difficult to apply uniformly, and the shape of the adherend Depending on the case, the adhesive sometimes protrudes.

  In addition, according to the inorganic adhesive, it is possible to form a uniform adhesive layer that does not foam, but it is desirable that the alkali metal is not contained in the semiconductor device member. I can't say that.

  The present invention has been made to solve the above technical problem, and is bonded with an adhesive layer that is uniform and free of bubbles, and has excellent adhesive strength at a high temperature of 200 ° C. or higher. In particular, an object of the present invention is to provide a method for producing a ceramic composite member that can be suitably used as a member for a plasma processing apparatus.

In the method for producing a ceramic composite material according to the present invention, a thermal fusion-type polyimide film having a thermal decomposition temperature of 300 ° C. or higher and a glass transition temperature of 180 ° C. or higher is provided between a ceramic substrate and a yttria ceramic sintered body. It is characterized in that an adhesive surface having a tensile strength of not less than 0.3 MPa at 250 ° C. or less is formed by pressing and heating between the layers.
By bonding a ceramic base material that is relatively easy to process and a yttria ceramic sintered body with excellent plasma resistance by the above method, an adhesive layer that is uniform and free of bubbles can be formed. Excellent adhesive strength can be obtained even at a high temperature of 200 ° C. or higher.

As the film, those obtained by applying a polyimide adhesive to the surface of a film substrate made of aromatic polyimide, or those made only of a polyimide adhesive are preferably used.
It is possible to form the adhesive layer in a uniform and bubble-free state by preliminarily forming a film to be thermally fused polyimide instead of a liquid adhesive.

As described above, according to the method for producing a ceramic composite material according to the present invention, a ceramic composite material that is bonded with an adhesive layer that is uniform and free of bubbles and has excellent adhesive strength at a high temperature of 200 ° C. or higher can be obtained. .
Therefore, the ceramic composite material can be suitably used as a member for a semiconductor / liquid crystal manufacturing apparatus or the like, particularly a plasma processing apparatus.
Further, in producing a plasma-resistant ceramic member, if the production method according to the present invention is used, the amount of yttria ceramics that are expensive and difficult to process complicated shapes can be suppressed. This is also advantageous in terms of cost.

Hereinafter, the present invention will be described in more detail.
In the method for producing a ceramic composite material according to the present invention, a thermal fusion-type polyimide film having a thermal decomposition temperature of 300 ° C. or higher and a glass transition temperature of 180 ° C. or higher is provided between a ceramic substrate and a yttria ceramic sintered body. The present invention relates to a method of adhering by pressurizing and heating.
As a result, a ceramic composite material in which the adhesive surface between the ceramic base material and the yttria ceramic sintered body has a tensile strength at 250 ° C. or less of 0.3 MPa or more is obtained.

That is, the ceramic composite material according to the present invention uses a heat-fusion type polyimide film excellent in heat resistance as an adhesive, and a yttria ceramic sintered excellent in plasma resistance on a ceramic substrate that is relatively easy to process. The body is joined.
By bonding ceramics by such a method, an adhesive layer that is uniform and free of bubbles can be formed, and excellent adhesive strength can be obtained even at a high temperature of 200 ° C. or higher.
In addition, if a ceramic composite material is manufactured by the above method, the amount of yttria ceramics that are expensive and difficult to process complicated shapes can be suppressed, which is advantageous in terms of cost.

The yttria ceramic is required to have a corrosion resistance against corrosive gas and plasma in order to be suitably used as a member for a semiconductor / liquid crystal manufacturing apparatus or the like, particularly a plasma processing apparatus. preferable.
Moreover, it is preferable to grind the joining surface of the ceramic base material and the yttria ceramic sintered body so that the surface roughness Ra is equal to or less than the thickness of the adhesive layer in order to increase the adhesive strength.

In addition, as the heat fusion type polyimide film used in the present invention, a film base material made of an aromatic polyimide with a polyimide adhesive applied thereto is preferably used. Alternatively, it may be composed only of a film-like polyimide adhesive.
In any case, in the present invention, the adhesive layer is formed in a uniform and bubble-free state by previously forming a polyimide film to be thermally fused instead of a liquid adhesive. It becomes possible.

Since the composite ceramic material according to the present invention is used at about 150 to 200 ° C. in a semiconductor manufacturing apparatus or the like, it is preferable that the polyimide film has a thermal decomposition temperature of 300 ° C. or more as an index of heat resistance. More preferably, it is 350 ° C. or higher.
The glass transition temperature is preferably 180 ° C. or higher, and more preferably 250 ° C. or higher.

When using a polyimide film composed of a film substrate and an adhesive, the film substrate adheres ceramics to each other. Therefore, it is preferable that there is no shrinkage due to heating, and a material having a low thermal expansion coefficient is suitable. Used.
The thickness of the film substrate is preferably 50 μm or less from the viewpoint of appearance.

Further, the thickness of the polyimide adhesive layer is preferably 1 μm or more, more preferably 10 μm or more, because the ground surfaces of the ceramic sintered bodies are bonded to each other.
The type of the polyimide-based adhesive is not particularly limited as long as it is heat-fusible and can be uniformly fused in the bonding surface by pressing and heating.

  The heating temperature at the time of bonding is appropriately set to a temperature at which the polyimide film is uniformly fused in the bonding surface, and the pressure at the time of bonding is determined in consideration of the strength of the ceramic sintered body that is the adherend. And adjusted as appropriate.

EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example, this invention is not restrict | limited by the following Example.
[Example]
A base material made of an alumina ceramic sintered body (purity 99.5%) and a yttria ceramic sintered body (purity 99.9%) were each subjected to 6-side surface grinding, and an adhesive surface 20 mm × 20 mm, surface roughness Ra 0.9 to 1.3 μm, Ry 7.9 to 11.1 μm).
Between these two test pieces, a heat-sealable polyimide film for a flexible printed circuit (FPC) substrate (Upilex VT manufactured by Ube Industries, Ltd .; thermal decomposition temperature: 350 to 400 ° C., glass transition temperature: 240 ° C.) The test pieces were sandwiched and bonded at a heating temperature of 350 ° C. and a pressure of 4.8 × 10 ⁻³ MPa.
The formed adhesive surface was uniform and the tensile strength at room temperature was 0.4 MPa.
In addition, the tensile strength in the heated state is 0.4 MPa up to 230 ° C., and decreases when it exceeds 270 ° C., and at 320 ° C., partial peeling is observed on the adhesive surface. 1 MPa.

The heating temperature in the case of 310 ° C. or less, applied pressure was not adhered in ^{1.2 × 10 -3 ~4.8 × 10 -3} MPa.
Further, when the heating temperature was 330 ° C., partial adhesion was recognized at a pressurization pressure of 4.8 × 10 ⁻³ MPa.

[Comparative example]
A test piece of a ceramic sintered body similar to that of the example was cured and bonded at room temperature using an epoxy adhesive.
The formed adhesive surface had a tensile strength at room temperature of 0.7 MPa, but peeled off when heated to 200 ° C.

Claims (2)

  Between a ceramic substrate and a yttria ceramic sintered body, a heat fusion type polyimide film having a thermal decomposition temperature of 300 ° C. or higher and a glass transition temperature of 180 ° C. or higher is sandwiched between the ceramic substrate and the yttria ceramic sintered body. A method for producing a ceramic composite material comprising forming an adhesive surface having a tensile strength of 0.3 MPa or more.   2. The ceramic composite material according to claim 1, wherein the film is formed by coating a polyimide-based adhesive on the surface of a film substrate made of an aromatic polyimide, or made of only a polyimide-based adhesive. 3. Manufacturing method.