JPS60180968A - Insert material for bonding nitride ceramic - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a bonding insert material for nitride ceramics, and particularly relates to a bonding insert material for nitride-based ceramics, and particularly for bonding inserts between St, N4, or Si.
It relates to an insert material used to join 3N4 and other metals.

Ceramic materials have made remarkable progress in recent years, and various ceramics with even higher performance have been developed using high-purity oxides, carbides, nitrides, borides, silicides, and the like as raw materials.

These are called new ceramics in contrast to conventional ceramics manufactured from natural raw materials, and are widely used in various fields such as heat resistance, electronic devices, and optics.

By the way, even in the new ceramics with various improved properties as described above, there is a common drawback of being weak against mechanical shock and thermal shock, and it is desired to eliminate this drawback. In order to compensate for this shortcoming and further expand the application fields of ceramics, ceramics can be used with other materials,
For example, it may be possible to bond with metal. At present, among new ceramics, various joining methods have been proposed and put into practical use for oxide ceramics. However, among the new ceramics, nitride-based ceramics, which are called fine ceramics, have a short history of development, so the joining method has not yet been established.

The present invention has been made in view of the above, and its purpose is to provide an insert material capable of joining nitride ceramics as described above, or nitride ceramics and metals such as Inconel, in good condition. It's about doing.

The insert material for bonding nitride-based ceramics of the present invention, which meets the above objectives, contains 20% to 70% Cr (weight ratio).
It is characterized by containing Fe and/or Ni in the remainder.

By interposing the insert material as described above between the surfaces to be joined,
10 to 10 Torr in vacuum or in an inert gas atmosphere, and slightly pressurized (0.2 to 0.3 Torr).
g / *: degree), the whole is 1300-135
By heating to 0℃ and melting the insert material,
Good joints can be obtained.

The reason why Cr is set to 20 to 70% (weight% and below is the same) is as follows.
If the Cr content is less than 20%, peeling cracks or incomplete melting will occur on the ceramic side, while if the Cr content exceeds 70%, the melting point will be extremely high, the reactivity will be poor, and a good This is because a joint cannot be obtained.

The remainder of the insert material is Fe within a range of 70% or less.
It is preferable to contain both Ni and Ni in the range of 5 to 70%, but either one may be used alone.

In addition, the remaining part of the insert material contains Fe and/or N.
It may contain other elements other than i, such as C, Ti, Nb, ■, AI, etc.

Next, regarding specific examples of the insert material of this invention,
This will be explained in detail with reference to the drawings.

This is because a bonding test was conducted using insert materials having various compositions, and the bonding conditions at that time will be explained first. In addition, the test piece was 5t with a diameter of Low and a length of 10 pieces.
) A round bar made of N4 was used.

First, an insert material with a thickness of about 10 to 50 μm is placed between the joint surfaces of the test piece, placed in a vacuum container at about 10 to 10 Torr, and a pressure of about 20 g is applied to the test piece. Load it. From this room temperature state, as shown in Figure 1, with a temperature increase time (Tl) of 2 to 3 hours,
Heat to 1300-1350°C.

Immediately after reaching this temperature, or after maintaining this temperature for an appropriate time (T2) within 2 hours, heating is stopped and the furnace is cooled. The cooling time (T3) in the furnace is about 5 hours. Note that the holding time at 1,300 to 1,350°C mentioned above may be zero, but in order to melt the insert material more reliably, it should be held for a predetermined period of time in consideration of the stability of the heating operation. It is preferable that
In addition, 1. Since no change in the bonded state is observed even if the holding time is longer than 2 hours, it is possible to hold the bond under heating for a long time, but considering work efficiency, it is recommended to hold the bond for a period of 2 hours or less. It is preferable that

FIG. 2 shows the results of a bonding test using insert materials having various components in the Cr-Wound-Fe system.

As shown in the figure, if the Cr content is less than 20%, peeling cracks will occur in the ceramic, and if the Cr content is more than 70%, incomplete melting will occur due to an increase in the melting point of the insert material. It is clear that Cr in the range of 20 to 70% shows relatively good results.

Figure 3 shows the components within the above range (Cr: 24%, N
Si3 was heated at a heating temperature of 1350°C and a holding time of 0 minutes using an insert material having
A microscopic photograph of the joint portion when N4 is connected to each other is shown. As shown in the figure, it is clear that a transition layer is formed between the ceramic and the insert material, resulting in a good connection. Further, FIG. 4 shows the test results of the shear strength of the above-mentioned joint, and it is clear from the figure that a relatively strong joint can be obtained.

Although the mechanism by which the transition layer is formed as described above and the specific distribution of components in the transition layer are not clear, it is possible that the aluminum oxide and potassium oxide contained in the ceramics diffuse into the insert. At the same time,
It has been confirmed that nickel diffuses into the ceramic side from the insert collapse, and that a relatively large amount of chromium exists at the boundary between the ceramic and the insert material.

Therefore, the above-mentioned bonding is performed by the above-mentioned mutual diffusion, and chromium nitride is further formed at the boundary, and chemical bonding between the ceramic and the insert material occurs through this chromium nitride. It is presumed that this is because it was carried out.

Table 1 lists other components other than Cr, Ni, and Fe (T
i.

The results of a bonding test using an insert material containing (Nb, V, AI) are shown. In the same table, O indicates that the bonding condition is good, and × indicates that the bonding condition is not good, but from the same table, it can be seen that other components are present in the insert material where Cr is the gatekeeper of the scope of the present invention. It is clear that a good bonding state can be obtained even if

In addition, the above insert material (Cr: 23.5%, Ni
: 24.5%, Fe: 48.5%, Ti: 2%,
Nb: 1.5%) at a heating temperature of 1300°C.
Figure 5 shows a microscopic photograph of the joint when ceramics are joined together with a holding time of 30 minutes, and Figure 6 shows the test results of the shear strength of the joint in that case. It is clear that a good bonding state can be obtained even when using an insert material having the following properties.

The embodiments of the insert material of the present invention have been described above, but
The insert material of the present invention is not limited to the above-mentioned embodiments, and can be implemented with various modifications. For example, in the above, the test results were shown in which ceramics (Si3N4) were joined together, but the insert material and Inc.
The bondability with metals such as onel 7L3C is good, and it has been confirmed that by interposing the above insert material between the ceramic and metal, a good bonding condition similar to the above can be obtained. . We have also confirmed that ingredients other than those listed above can be added to the insert material, and that even if the insert material contains some unavoidable impurities such as C, its performance will not be affected. There is.

The insert material for bonding nitride-based ceramics of the present invention is constructed as described above, and therefore, by using the insert material of the present invention, it is possible to bond nitride-based ceramics, which has conventionally been considered impossible. , they can be joined to each other or to other metals.

[Brief explanation of the drawing]

Fig. 1 is a graph showing the temperature history in the bonding method using the insert material of the present invention, and Fig. 2 is a graph showing the Cr-Nr-Fe ternary system percentage to show an example of the component range of the insert material of the present invention. Figure 3 is a diagram showing the metallographic structure of a joint using the above insert material, Figure 4 is a graph showing the test results of the shear strength of the joint, and Figure 5 is a diagram showing the metallographic structure of a joint using the above insert material. FIG. 6 is a diagram showing the metal structure of the joint used, and a graph showing the test results of the shear strength of the joint.

Claims (1)

[Claims] 1. An insert material for joining nitride-based ceramics, which contains 20% to 70% (weight ratio) of Cr, and further contains Fe and/or Ni in the balance.