JPS58151376A - Adhesive for ceramics and adhesion - 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 cefmix adhesive and a method for adhering the same, and particularly relates to a Cefmix adhesive and a method for adhering the same, and particularly relates to a Cefmix adhesive and a method for adhering the same, and particularly relates to a cefmix adhesive and a method for adhering the same, and in particular to 'iIli silicon, silicon carbide, nylon◆O#p
A mixture of sulfides and other ceramic materials! , fK￥＠I am grateful for the good luck copying agents and their adhesion methods.

Non-oxide ceramics such as silicon carbide, silicon nitride, and NIARO ν are new and different from metal oxide ceramic materials because of their excellent strength, tI# impact resistance, and chemical resistance. In recent years, it has been in the spotlight as a high-temperature resistant material, and various applications are being made. Once you get the hang of it, these ingredients are Karasmen I&-1 Kosei 111! mechanical parts,
The development of its use in heat exchangers, etc., as magnetic parts with high IK, and as special high-temperature insulators is being considered.

In order to utilize these non-oxide ceramics and fully demonstrate their characteristics, Kl-! In the manufacturing process of various devices and their parts, it is necessary to bond non-oxide ceramics to each other or to other materials, and in particular, bonding technology for oxide ceramics formed into various shapes is required. development is essential.

However, non-oxide ceramics generally have extremely poor demand for steel due to their affinity for molten materials, and unlike metal oxide ceramic materials such as alumina and magnesia◆, they have strong covalent bonds, and other Its reactivity with compounds is also very low, and its coefficient of thermal expansion is less than half that of alumina, making it extremely difficult to bond. In fact, conventionally, the only known method for adhering the fluoride thread ceramics is the hot press method under high temperature and pressure. The bonding strength of the material is extremely difficult, and even if it can be removed by itself, the adhesive strength is still insufficient.

Considering the current state of K11l mentioned above, the present inventors have found that it is possible to easily increase the size of the IMl under milder conditions without using the hot press method.
Various studies were conducted in order to develop a new vibrating agent warp bonding method that can bond materials of irregular shapes with sufficient adhesive strength. However, in the case of Joki Non-Abrasive A Ceramics Adhesive K,
Not only does it have the feature of being able to be removed with sufficient adhesive force, but the adhesive layer itself that is formed is chemically stable, and it does not have any negative effects on the characteristics of the It has been found that the adhesives and adhesives currently known have excellent heat resistance, thermal shock resistance, etc., to the extent that they do not deteriorate, and do not have the above-mentioned properties. In subsequent research, the present inventors found w#
In addition, sodium fluoride and (also Fi)calcicum 7 fluoride are included in the Joki SeikatX, and these are suitable for bonding not only Fi fluoride oxide-based mixes but also shrimp-based ceramics. Based on this discovery, he has perfected his invention and has already filed an application. The adhesive related to this release 1j4 is extremely excellent, and in the process of investigating its application fields, we discovered the following new fact. That is, (a) alkali metal heptafluorides and alkaline earth metal heptafluorides other than the above-mentioned sodium fluoride and rough calcium heptafluoride exhibit similar effects; (b) alkali metal fluoride (sodium fluoride) (including However, depending on the place where the pinhole is used, it is not necessarily considered to be fr black if the pinhole causes an unexpected adverse effect on the adhesive. It has been discovered that the prevention can be efficiently prevented by allowing at least one type of alkaline earth-metal compound to coexist.The present invention was completed based on these detailed discoveries. That is, the present invention provides an adhesive for bonding ceramics containing as active ingredients at least one of ittria and alkaline earth metal compounds (excluding heptadides), an alkali metal fluoride, or a mixture of these and kaolin; Adhesives containing as active ingredients at least one of ittria and alkaline earth metal compounds (excluding heptadides), alkali gold fluoride, or a mixture of these and kaolin can be used to bond non-oxide ceramics. A method characterized by interposing the oxide thread ceramics between the oxide thread ceramics or between the non-saponifiable thread ceramics and the oxide ceramics, and heating them above the decomposition temperature of the 7 fluoride. This is related to the method of adhering the mix.

The adhesive of the present invention excludes yttria and alkaline earth metal compounds (7). ) at least 1 yuzu and alkali gold w
47 fluoride as an active ingredient, but it may further contain kaolin or (and) an alkaline earth metal fluoride.

These lids can be used in any case without being specified by lI#, but they contain 20 to 80 mm% of at least one of itria and alkaline earth metal compounds and alkali metal fluoride. Monster is 20~SOW%, Kaolin #
'i (and) alkaline earth metal fluoride is 0 to 60]1
The amount is %.

The adhesive of the present invention has this ratio #l! The temperature is usually about 1000 to 1500°C, preferably about 10
By simply decorating at 00 to 1300°C, ceramics can be easily bonded without any pressure or pinholes. When cooking, as the amount of alkali gold lI47tsubide 0111J in the wk appetizer increases, it becomes possible to cook at a lower temperature within the above heating range.

The initial adhesive has the great advantage of being able to bond especially fluoride thread ceramics;
*Ashes are more than M400/d, 4/l- to 600
It is about 300&#/C by the known method.
At the limit of m, it is possible to achieve an improvement of about 30% or more, twice as much as compared to Metsu9. To the east, the adhesive of the present invention can be applied to complex oxide-based sexics materials that cannot be Fi** using known methods!
ME can also be applied to Ik clothes, and the material IP+ can also be strongly inspected. In addition, the adhesive of the present invention is advantageous in that the adhesive layer is chemically stable and has a heat resistance that is suitable for use with non-oxide ceramics.
Has thermal shock resistance.

The use of the adhesive of the present invention to bring about the various outstanding effects mentioned above is not currently in use, but the following ideas can be considered. That is, the alkali metal heptafluoride constituting the adhesive of the present invention, or the alkali metal heptafluoride and the alkaline earth gold fluoride, are mixed between non-oxide ceramics, between oxide ceramics, or between non-oxide ceramics and graded yarn. By interposing the fluorine gas between the ceramic material and heating it to a temperature higher than the decomposition humidity, it decomposes and generates fluorine gas. A metal or a reaction product of this and an alkaline earth metal, or a reaction product of these and kaolin,
It is thought that the adhesive penetrates into the eroded material as described above and forms an adhesive layer having an adhesive force t- that contributes to the adhered material N (b). In the case of Zero-Hatsu #1 adhesive containing kaolin, the kaolin activates the alkali metals and/or alkaline earth metals generated by the heating, further promoting their penetration into the ceramic material. It seems to be possible to do so. 4kIfi rent % see the heron ζ beak ＼
~ Heichi to Ken ~ From Noodle Cover to Sukadakabei ~ % ~ ~ At this time, in the present invention, due to the presence of ittria and (also) alkaline earth metal compounds, alkali metal heptadides are enriched. Examples of non-oxide ceramics to which the present adhesive is applied include silicon carbide, silicon nitride, and sialon. It should be noted that these are nitrides of sialon, silicon, and aluminum. These '#W between oxides
An example of kS is silicon carbide - silicon carbide, silicon nitride -
Examples include adhesion between silicon nitride, silicon nitride-silicon carbide, nitride-nylon, silicon carbide-sialon, and sialon-sialon.

In addition, the adhesive of the present invention can be used in combination with the above-mentioned non-oxide ceramics and natural ceramics such as alumina, mullite ceramics, zirconia, beryllia, cordierite, etc.
Bond with Magnej 1st class, f or above! It is also suitable for adhesion between # compound yarn ceramics.

Gold can also be bonded to a non-oxide ceramic thread through the oxide ceramic thread. in this case#
Since the properties of fluoride ceramics and metals are very different, oxide thread ceramics are provided between them. If the thickness of this oxide ceramic is less than 5 mm, it is sufficient to use only one cypress, but if the thickness is greater than 5 fl, it is treated as an oxide ceramic with an expansion coefficient of 211 or more. It is preferable to use different ones in combination. In this case, gold includes a wide variety of materials.

These non-oxide-based, oxide-based, or gilt-copper materials are not particularly limited in shape or size, and may have any shape such as a plate, column, pipe, or block, and can be bonded to The materials to be used may have the same shape or different shapes.

Examples of the alkaline fluoride used as an active ingredient in the adhesive of the present invention include lyticum heptafluoride, calicum fluoride, sodium heptafluoride, rubidicum heptafluoride, and alkaline soils that are used as necessary KI15. Examples of similar metal heptafluorides include perilicum heptafluoride, calcium heptafluoride, magnesium fluoride, stronticum fluoride, and palicum fluoride.

The purity of these heptafluorides is not particularly limited, but in order to increase adhesive strength, it is preferable that the purity is as high as possible. In addition, alkaline earth metal compounds that may be used in the present invention include oxidized lucicum, saponified magnesium, perilicum oxide, varicum oxide, stronticum oxide, and other oxides, as well as calcium carbonate, saponified magnesium, berylicum, paricum, and carbonic acid. Carbonated compounds such as stronticum etc.'4! : Can be illustrated as an example of J4 body.

This ◆ Alkaline pot III + 7 fluoride, alkaline earth metal heptadide, ittria and alkaline earth gold w4 fluoride are Jlkt II! It is advantageously used in the available powdered form. Any commercially available kaolin can be used, especially the production area (YA Ishino & Aku),
It is not limited to the crystal size, history, etc. Its composition is mainly composed of 5ins and Als Os, and Fe1 as well.
O@, Ti01. You can use a self-produced one that contains a small amount of CaO1K, O, etc., but it is better to use one with a higher purity because it will produce alkali gold-7 fluoride and alkaline earth gold w47.
It is expected that the adhesive strength of tsunide can be higher than t. It can also improve the physical properties of post-mortem nursing pigeons.

The adhesive of the present invention contains at least 1a of the above-mentioned IJA and an alkaline earth metal compound [and alkali gold W47].
) compound or a mixed powder made by simply mixing these with kaolin or alkaline earth metal fluoride (and) alkaline earth metal fluoride. It can also be used in the form of a paste or the like by blending it with a substance or a solvent.

This is how you get a book! In its use, the i1A attracting field agent is introduced into the mass of material to be removed and then heated to a temperature sufficient to decompose the alkali metal fluoride or alkaline earth metal fluoride. Here, the application of the adhesive of the present invention to the amount of material is as follows: if the adhesive is in powder form, it is sufficient to apply it to the recipient 1]K*; For adhesives of 1**, Km can be added in the same way as the adhesive in item 1**. The application method is determined as appropriate depending on the composition of the tIk agent used, especially the amount of kaolin used, the heating conditions after applying the agent, and the seed koji and shape of the material to be welded. Preferably, about 1-1 g of FiO is applied to #4 adhesive from Kakuma Publishing Co., Ltd. after applying the adhesive as described above. The temperature may be set so that the earth metal fluoride decomposes and releases 7'Jk.

In the present invention, it is not necessary to employ any pressure means when applying Fi, especially the above-mentioned IK, but it is possible to apply some pressure to ensure the softness of the adherend L. In addition, the above heating is generally performed at 22! Although it can be easily carried out in air, if there is a risk of oxidation due to addition of the adhesive material, it can also be carried out under a nitrogen atmosphere.

A ninth example will be given below to further explain the present invention.

Example 1 Silicon nitride plate and Mukuite ceramics & (Nipponkaji part'
V! During production, a mixed powder consisting of 30% Lia and 70% Sodium chloride was sprinkled at a rate of 0.5g per 1m in the horizontal direction, and a muquitous semix board was added. Place a copper plate on top and heat it in an electric furnace for 110 minutes.
Heated at 0°C for 20 minutes.

The magnetic strength of the obtained post-mortem composite sample was determined according to the three-point coulometric strength measurement method under the conditions of Span 2011 and a loading speed of 0.5 cm/-, and was found to be 470 kf/d.

In addition, after the above measurement, the vertical direction is as shown below. It was destroyed by L.

Part II: All samples of the jointed joints were immersed in a potassium hydroxide solution for 70 hours at 70°C to examine their chemical resistance. Good luck.

In a quenching test in which the above-mentioned cathedral body was heated to 1100°C and then quenched in the air, it was found to have K4 heat resistance at the chest area, and no certificate of merit was found on the adhesive part.

Investigation & Examples 2 to 4 In Example 4M11, the blending ratio of ittria powder and sodium heptafluoride powder was made more cypress to create the present invention + jk agent, and using these, silicon nitride was prepared in the same manner: ik!
1 Mukuito II [Cefmix board - Glue the copper plate 9.

The adhesive strength, chemical resistance and IIN heat III properties of each of the borrowed bonded bodies 1KII+ were measured in the same manner as in Example 1, and the results are shown in Table 1 below.

Table 1 *Example S Ittria sO weight % and sodium heptadide? 011m
Mixed powder from m to 3 pieces of powder
, insert a piece of cloth in the amount sg, and check the ξ angle with the hook l and the ladder K.
Heat at 100°C for 10 minutes and wait for conjugate 1. After death, add O adhesive strength to fIja and key points, 6104/
d was good, and there were no deviations in the resistance to adhesion and thermal shock when subjected to IK. 1 Examples 6 to 1 In Soap Example S, the blending ratio of Ittria powder and roughened Natrichum hI wood was varied to make Kiwagawa adhesive f'
Using these materials, two sheets of nitrided carbon fiber were similarly shaken, and the Tsukuda IIj 1 degree, wheel resistance, and skin impact resistance of each of the obtained bonded materials were evaluated as in Example 1. The M result obtained by 1nalK is shown in the cram school table 2 below.

Table 3 *ia Example 9 Mixed powder tMI consisting of 7000 calcicum and 30 irises was added to Nihon Kagaku 4M (41011 ceramic). , Example 1 and I11 were prepared and three points about the nine tests I
It was #I〆 and nine knots, hlo pass / d.

Music resistance and crucian carp a were made according to Jil1MIK on the pipe.
SS was rarely diagnosed without any abnormalities.

Examples 1O to 13 In Example 9, various blending ratios of calcium oxide and sodium fluoride were used to create adhesives, and these were used to uniformly coat silicon nitride plates. Table 3 below shows the results of the noodle strength, Qin resistance, and crucian carp attack resistance of each monk El') borrowed from Example 1 and 11K. .

Table 3 Example 14 A mixed powder consisting of oxidizing power Rusicum 30] 11L lid% and 70 tons m* of Sodium heptase was placed between two sheets of Lucicum &l.
- Todoroki o, interpose the front cloth in the grave called sg, and this is an example 1
The grudge strength of the zygote sample obtained by heating in
It was sao#/d. In addition, in the same tests as in Example 1, there was no grade 4A in both the elasticity resistance and thermal shock resistance.

A zero-invention sprinkling agent was created by changing the blending ratio of oxidizing power lucicum and sodium fluoride in Shinshi-JIS ~ 17 Shinshi-+14, and these tF@ and -m were coated with two plates of silicon nitride-Tao Shishin. Made of wood
Table 4 shows the results of the determination of the degree of bond, quality and heat shock resistance of each loss-combined vehicle for the following cases: Example 1 and Example 1.

Table 4 Example 18 A mixed powder consisting of 80% calcicum and 7% calcicum was placed between a silicon nitride board and a sekmic board at a concentration of 0.5 g per 1kIIItl. At the foot of the mountain, the copper plate was sprinkled on top of the mullite ceramic plate, and this was heated at 1100℃ for 20 minutes in a VT furnace.
Heated for minutes.

The 1 degree per click of the obtained zygote sample was measured according to Example 1, and it was found to be 5504/d. Also, the same 1i1 as in Example 1
No abnormalities were found in both chemical resistance and impact resistance.

(that's all)

Claims (1)

[Scope of Claims] 1. Ittria and alkaline earth metal compounds (7tria)
Excluding e. ), as well as a mixture of a chilled metal fluoride, a filament, etc., and kaolin as active ingredients. 2. Patent claim #Q in which the alkaline earth metal compound is an alkaline earth metal plating or an alkaline earth gold X-translated oxide
Adhesive described in the first product. 8. $1 of the patent claim in which the ceramic is non-oxide based
1$$ I JJ4 D description f) M meeting M. 4. The adhesive according to claim 4, wherein the fluorinated Il#j ceramic is at least 1fI of silicon carbide, silicon nitride, and nylon. b. The adhesive according to claim 1, wherein the ceramic is oxide-based. 6. Excludes ittria and alkaline earth metal compounds (7). ) and an alkali metal heptadide, or a mixture of ξ ◆ and kaolin, as an active ingredient. and an oxide thread ceramic, which is heated to a temperature higher than the decomposition temperature of the heptafluoride. 7. Non-oxide thread ceramics, oxide thread ceramics, and other oxide thread ceramics having a larger expansion coefficient than the oxide-based ceramics are laminated in this order with the adhesive interposed between them. 17. The conventional method of claim 16. 8. The bonding method according to claim 4@1, item 7, wherein the oxide thread ceramic having a large expansion coefficient has a metal bonded in advance to one surface thereof.