DE1953891A1 - Putty material - Google Patents

Description

F. PHN.

Va / WG

Ϊ-ΪΗΝ-3743
10/23/69

"Putty material"

The invention relates to a cement material, in particular for use in cement connections between metal and a ceramic material, between two metals or between two ceramic materials.

Such putty connections are often high operating temperatures during the operation of the devices in which they are used exposed and it is desirable to manufacture them at relatively low temperatures, so that any change in the components is avoided (deformation, Brittleness, etc.).

It is known , iir putty connections between

a ceramic material and metal or between C-las and Metal to use stable types of glass belonging to the type of so-called "long" types of glass, i.e. types of glass,

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BATH ORIGINAL

-2- F. PHN. 37 ^ 3

whose viscosity remains high over a wide temperature range and whose silicon content is high.

The adhesion between (! Las and metal is brought about by a chemical bond that is obtained by the oxide layer remaining between the material and the glass after cementing; a "long" type of glass which is used in the case of d < ι for the production of the Putty compound required temperature> n has a high viscosity, makes it difficult to dissolve the oxide layer.

In connection with the wide temperature range, in which the viscosity of such Ki compounds sir · ι but will be the maximum operating temperature of the devices in which these putty compounds are applied far below that Putty temperature.

Also is the composition of a glass of this type such that its specific resistance decreases rapidly as the temperature increases.

US Pat. No. 3,113,878 describes a cement material which is composed of ontfflasable cilas of the "short" type with a relatively low silicon content. The composition of these described glass types. is such that the sum of the three oxides ZnO + B ₀ O + J is at least 90 $. However, these compositions have a high ZnO content, so that the range of expansion coefficients of the different types of glass is relatively narrow , which limits the possible uses.

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-3- F. PHN. 37 ¹ O

The purpose of the invention is to provide a new putty material that can be used for many purposes, in particular at higher temperatures, can be used, with direfavorable Maintain mechanical and electrical properties will.

The invention relates to a new cement material, in particular for the production of a connection between materials whose coefficient of expansion is between approximately '4 3 and U) O. 10 ~ '/ ° C, which cement material consists of a devitrifiable glass of the "short""type based on the oxides of aluminum, boron, silicon, zinc and possibly cadmium and which also contains oxides, the netzwerkändi -, idc ions supply, such as alkaline oxide or "magnesium," where the mentioned material is characterized in that the amounts of the starting components in moles are within the following limits:

SiO _r , ο - 2b

B ₀ O ₃ . 9 - 36

ΑΙ., Ο ο - 16

CaO + SrO + BaO + Mgo < > - 5b

/ lid + (ΙIu η _ -, {.

where the sum of CaO + Sr- t- BaO + MgO + ZnO + CdO is equal or greater than 50 moles. ^

fcegen their high content of network changing Ions attack this (ilasarten the oxide layer that the Adhesion between the glass and the metal causes only a small degree of .. For example, in the following Table of different starting compositions of putty materials given according to the invention:?

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ORIGINAL

F. PHN. 3743

I.
Number O 1 - 2 j 57 3 I. to
4 5 velvet
6th I. 69 netsetzun ¹ 70 8th 9 I. 10 I. ii M
ι—
1 1 12th 13th ί 14th i 15th —R • 99 ^D 2 ° 3 ³⁵ 15th 10 15th 15th )
o 1
ί 35 15 15th 7th 15th 15th 7k
I.
I. 15th I.
76
i 35 15th 15th I.
I.
83 ' 20th 86 ' 15th 16 . SiO ₂ 10 20th 20th 20th 10 20 20th ³⁵ 20th 20th 20th 10 20th 20th 15th 20th 15th ί Al ₂ O ₃ 5 5 5 10 5 10 15th 15th j CaO 5
j 50 15, 20 20 20th 25th 25th 25th 45 4o j SrO
j 25th 40 55 ί BaO:
I ί 53 25th ■ MgO 5 ί ZnO ■ 50 45 50 35 4oi
ί 45 35 4o 35 30th IO 4o 10 25th ^; io? 30th 10 between j
20 and j 47
32O ° C j 64 65 72 80 ^; 82 90

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In certain cases it can be beneficial if at least part of the zinc oxide is replaced by cadmium oxide will.

Z.H. the zinc oxide of compositions 5 and 7 at $ 50 can be replaced by cadmium oxide.

These compositions correspond to devitrifiable Short type glasses, borosilicate systems and borosilico zinc aluminate systems and alkaline earth ions, which if they are a contain a sufficient number of network-changing ions, di ;; zui ' Keep the oxide layer required to make a good connection. They are made according to the well-known Glastechn'.k machined at temperatures between 1200 and 1450 C.

The resulting molten glass is then converted into a frit, e.g. by placing it in water is hardened, after which it is ground; it can then be used as cement material. The putty connection will manufactured by the usual techniques in an atmosphere that depends on the nature of the interconnected Parts is selected and set.

Due to the selected starting composition and the fine distribution of the ground cement, the glasses are converted into glass kerosene products, which consist of a vitreous network in which there are finely divided microcrystals of one or more crystal phases. The presence of the latter has a beneficial effect on the mechanical properties of the compound. The content of crystal phase, which is from the starting

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composition and temperature, called the compound is made is dependent, but must remain low in order to achieve that the material is between the seams of the Parts to be connected to one another can i'liessen.

The time and the temperature of the production of the cement connection are therefore not only dependent on the type of parts to be connected, but also in Dependence on its geometry, its wetting properties and their flow chosen.

The mechanical properties of the obtained

Connections that are determined by the flexural strength. ¹ , are given below for various experiments in which certain compositions of Table 1 are used.

The initial composition is chosen in such a way that the expansion coefficient of the cement material is matched to that of the bodies to be connected. The conditions under which the connections are made are determined by the duration and temperature. example 1

With the help of PuIv rn with compositions O,

1, 2, k, 5, 6, 7 and 9 according to de Table 1, cylindrical test tubes from Ferniro are soldered together in a nitrogen atmosphere containing 25 tfassersto, ί and saturated with water vapor at room temperature.

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F. PHN. 37 ^ 3

Together-
punishment i 0 ; ι ^; 2 . k 5 6th 900 9 treatment
10 minutes at t
; 950 ; 1100 1030 t
950 1050 1100 10.3 10 50 Bending
strength
in kg / mm-2 I.
'18, 1 10.1 17.5 18 1 21.9 18.2 8th

The * flexural strength is still high,

even if the expansion coefficient of the connection differs from that of the material to be connected. From a mechanical point of view, excellent results are achieved with putty materials with a coefficient of expansion between ^ 7 and 69. 1O "'lie.
Example 2

With the aid of the compositions I ₁ 2, 3i 5i <J and 9, cylindrical test tubes made of sintered aluminum oxide are cemented to one another with their end faces in a non-reducing atmosphere.

composition

3 ι k

Treatment ; 10 minutes at j 1100

1050 .1100 '950 1050

1100 1050

I bending

_; strength 20.9 ■ 1b, 8 29.3 28.0 27.9 ^! 27.8; 19th

in kg / mm " ² ,

In fact, it is the inherent strength of the connection bigger than most of the ones carried out

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F. PHN. 37 ^ 3

Experiments, especially with the compositions 3 »+» 5 and 6, occurred in the aluminum oxide fracture. Example 3

With the aid of the compositions 1, 2, 3t ^ "5" and 9 cylindrical Aluminiumoxydringe saturated nitrogen atmosphere were soldered to cylindrical Fernicoringen in a 25 $ hydrogen-containing and with steam at room temperature.

■ Together
settlement 1 0 1050 3 H 0 , 5 6th 9 Treatment
temp. in ° C 100 , 0 1100 900 1050 1100 1050 Bending
strength
in kg / mm "" ^ j 22
I.
I. 16.5 y
j
ί 16, 16.3 1k, 3 13.1

The electrical properties of the connections, determined by the resistivity as a function of temperature are given in the table below, taking measurements with FerniCo connections on Fernico with the help of putty materials according to the invention with some Compositions of Table 1 were carried out.

In the last column, comparative

the results of the measurements of the resistivity of Fernico connections on Fernico with the help of a glass of the long type applied. In these compounds, the specific resistance increases a lot with increasing temperature faster to.

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BAt) ORIGINAL

F. PHN. 37 ^ 3

material

. 6th

.Glass from the "lance" I type

Manufacturing temperature: KJOO j 1050 in oc!

J1100

950

950

j measuring temperature j door in ⁰ C

j 300 • 350

1, k Log. of the spec • Resistance in J. .cm 1 j 1 O - 11.2 y 8th, 6th i 1 9, 1 1 1 11.5; 10.0; 7, 10 ' 10.5 10 , 7 8.9 ^: -

45c »500 550 600 650 700

8.2

! ^{7> k}

I 6.9

I 6.5

j 6.2

9.1! 9.6 j 9.8 8.0:

8th, 2 I ⁸ ,8th 9, 0 7, 3 7, 8th ,1 8th, 3 6, 6th 6, 9 7th , 5 7, 7th 6, 0 - 7th , 0 7, 2 - - 6th , 0 6, 1 -

example k

For example, some of the above-mentioned Materials cemented together parts in the enclosed Drawings shown. Show it:

Fig. 1 Connections at a high-voltage breakdown

"-ung
there was a connection 1 between metal and metal, a connection 2 between metal and aluminum oxide, and a connection 3 between aluminum oxide and metal;

2 shows a connection k between a window 5

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BATH ORIGINAL

made of corundum and a Fernico frame ö, and

3 shows a connection "7" between metal 8

and alumina 9, being the different compounds were vacuum-tight.

0 0 9 8 2 1/16 9 2 ^{BAD 0RiGINAL}

Claims (1)

-11- F. PHN. 37 ^ 3 Patent entitlement ; Putty material, in particular for use in the production of connections between materials with a coefficient of expansion between approximately k * j and 100.10 / C, which is made of devitrifiable glass of the "short" type based on the oxides of aluminum, boron, silicon, zinc and possibly tadmium and which also contains oxides that supply network-changing ions, such as alkaline earth oxide or magnesium, characterized by the? the composition in moles £ is within the following limits: SiO ,, «9-26 B ₃ O ₃ 9-3O Al ₂ O ₃ 0-16 CaO + SrO + BaO + MgO 9-56 ZnO + CdO 9-5b, where the sum of CaO + SrO + BaO + MgO + ZnO + CdO is equal to or greater than 30 mol. ', V> is. 009321/1692 Blank page