DE102009005673A1 - Preparing beryllium containing mother alloy e.g. aluminum-beryllium alloy, useful e.g. in gas turbine engines, comprises converting a solid material mixture of a raw material comprising a beryllium concentrate and a metal component - Google Patents

Abstract

Preparation of a beryllium containing mother alloy comprises converting a solid material mixture of a raw material comprising a beryllium concentrate and a metal component in a temperature. Independent claims are included for: (1) mother alloy obtained by the above process and comprising a composition (I) containing 50-85 wt.% of aluminum, 1-5 wt.% of beryllium, 2x 10 ->8>to 1x 10 ->5>wt.% of oxygen, 3-40 wt.% of silicon and 0.5-5 wt.% of carbon, and a composition (II) containing 2-15 wt.% of aluminum, 1-5 wt.% of beryllium, 50-85 wt.% of metal, 2x 10 ->8>to 1x 10 ->5>wt.% of oxygen, 5-35 wt.% of silicon and 0.5-5 wt.% of carbon, where metal is chromium, nickel or copper; (2) the preparation of a beryllium-containing alloy comprising segregation of the mother alloy; and (3) an alloy from the preparation of a beryllium-containing alloy comprising a composition (III) containing 70-97 wt.% of aluminum, 1.5-3.5 wt.% of beryllium, less than 2x 10 ->8>wt.% of oxygen, 1-30 wt.% of silicon and less than 0.5 wt.% of carbon and a composition (IV) containing 4-12 wt.% of aluminum, 2-5 wt.% of beryllium, 60-85 wt.% of metal, less than 2x 10 ->8>wt.% of oxygen, 1-30 wt.% of silicon and less than 0.5 wt.% of carbon, where the metal is chromium, nickel or copper.

Description

The The present invention relates to a process for the preparation of a Beryllium-containing alloy, which is characterized in that a solid mixture comprising the ore beryl and a metal component, in the heat is converted to a beryllium-containing alloy. In addition concerns the present invention is a beryllium-containing alloy.

beryllium is a light metal, which in elemental form very hard and brittle is. Due to its position in the periodic table it has none classical properties of metals more, but rather represents a transition to the refractory elements boron and carbon. Therefore it has a remarkably high melting point, a very high Heat capacity and a a third higher modulus of elasticity as steel. In addition, it has a high vibration damping.

by virtue of beryllium is usually used as an alloying additive used. Copper beryllium, nickel beryllium and aluminum beryllium alloys are known, inter alia. Compared increased to the respective pure metal the addition of beryllium to the tensile strength, resulting in the use of such alloys makes it very versatile.

So offer z. B. copper beryllium alloys combination options of mechanical and electrical properties that are in their scope unique in copper alloys. The achievable after curing mechanical Strength is the highest all copper alloys, with at the same time an electrical conductivity is achieved, the higher is as the one of bronze. Such alloys are used for example in used in connection technology, electrical engineering and watchmaking. Because of his extraordinary high elasticity and its high conductivity one uses copper beryllium alloys also for heavily loaded Springs in movements and machines, electrical contacts, Overhead lines of road and railways, for sparkless tools and other.

In Extreme cases, in which the spring properties are maintained even at high temperatures is to remain is the nickel-beryllium alloy often the best solution because it has a high melting point. In addition, these alloys also in electrical contacts, electrical connectors, Diaphragms and compensating elements used. Because of the extreme high hardness and corrosion resistance become nickel-beryllium alloys also used in surgical instruments.

Aluminum-Beryllium have better physical and mechanical properties than classical ones Aluminum alloys. So they are characterized by a high mechanical Stability, high sound insulation and thermal conductivity and low weight. For aluminum beryllium alloys high modulus and low density of beryllium with the strength, Extensibility and the processing properties of aluminum combined. Because of these properties, aluminum beryllium alloys are used in gas turbine engines, Racecars, the aerospace industry and satellites used. In addition, aluminum-beryllium alloys find a wide Application for the protection of aluminum-magnesium alloys against oxidation.

The breadth of applications of beryllium in alloys shows that the currently high demand for beryllium will increase in the future. It will therefore be of great interest to provide new processes for the production of beryllium-containing alloys, which permit the production of beryllium alloys directly from beryllium concentrate, ensure a high yield of beryllium, and allow a cost reduction. Typically, beryllium-containing alloys are obtained by mixing and tempering beryllium with one or more particular metals. Normally, in the production of beryllium alloys from an ore, a beryllium compound (BeO, BeF ₂ , BeCl ₂ , etc.) is always first obtained by wet-chemical processes. From the compound thus prepared, electrochemical Be is produced which is used to produce an alloy. From manufactured pure BeO and BeF ₂ z. As well as Cu-Be alloys are obtained directly on carbothermic or metallothermal ways. These procedures are costly and inefficient.

It Therefore, an object of the present invention is a simple one To provide a method for producing beryllium-containing alloys, that makes it possible without complicated wet-chemical processes Be compounds for the reduction process directly from Be concentrate a Be alloy with controllable Si content, independent of the Si content of the concentrate is to win, and cost-effective and is efficient, and also ensures a high yield of beryllium.

A Another object of the present invention is to beryllium alloys provide, in addition to the desired metals certain proportions include aluminum and silicon, without that, in comparison with the "pure" alloys, the desired Properties are lost, or deteriorated to an extent that they are useless.

The above object according to the invention is achieved by a process for producing a beryllium-containing (pre) alloy, which comprises the following process step:
Reacting a solid mixture of starting materials at a temperature sufficient to form a beryllium-containing alloy, the solid mixture of starting materials comprising a beryllium concentrate and a metal component.

The Contains solid mixture preferably in addition Carbon. Carbon in the form of charcoal is preferred here used. In this case, the beryllium concentrate of the solid mixture of the reduction subjected to carbon.

Under a beryllium-containing alloy is understood in terms of this Invention any alloy containing beryllium as the metal component includes. Preference is given to alloys containing beryllium in the range of 0.1 to 20 masses, based on the total mass of the alloy. By master alloy is meant herein an alloy, the z. B. through seers to another alloy composition on can be processed.

In the present invention, beryllium concentrate is understood as meaning a naturally occurring beryllium-containing ore. The beryllium ore is preferably used. By the ore beryll one understands a solid with the composition Be ₃ Al ₂ Si ₆ O ₁₈ . The term metal component includes elemental metal, metal salts, such as. As metal carbonates, and metal oxides.

Of Further, it is preferred that the reaction of the starting materials at a temperature in the range of 1700 to 2300 ° C, preferably, 1800 to 2280 ° C, more preferably, 1900 to 2260 ° C, particularly preferably 2000 to 2240 ° C and extraordinary preferably 2090 to 2210 ° C. At temperatures below the specified minimum value, the reaction is incomplete, d. H. it does not find complete Reduction of the ore instead. This leads to unsatisfactory Exploit. For values above the specified range also take the alloy yields.

The metal component is preferably selected from the group consisting of the metals aluminum, chromium, nickel and copper, NiCO ₃ , CuCO ₃ , Al ₂ O ₃ , CrO ₂ , CrO ₃ , Cr ₂ O ₃ , NiO, Ni ₂ O ₃ , CuO, Cu ₂ O and mixtures thereof. Preference is given to using the metals or their oxides, particularly preferably the metals.

The mass ratio of the ore beryl to metal in the metal component is preferably in the range of 3/1 to 1/5, more preferably in the range of 2/1 to 1/4, even stronger preferably in the range of 1.5 / 1 to 1/3 and most preferably in the Range from 1 to 1 / 2.5. In the case of the use of aluminum or Aluminum oxide as a metal component is the ratio of ore beryll to aluminum in the range of 1/2 to 1/3 particularly preferred. In the case of use of copper as a metal component is the ratio of ore beryll to copper in the range of 1/1 to 1/2 particularly preferred. For metal contents below and above the given values decreases the metal and Beryllium yield in the alloy drastically. Within the specified Receives limits the maximum alloy yield and also the yield of beryllium in the alloy.

The mass ratio Carbon / beryllium concentrate is preferably in the range of To choose 3/10 to 3/1, more preferably 3.5 / 10 to 2/1, and most preferably 4/10 to 1.1. Below the specified range there is only an incomplete reduction instead of. A content of carbon above the stated ratio leads to an undesirable Carbon content in the alloy, d. H. deteriorates the alloy quality.

In the process according to the invention, the reducing agent serves to reduce beryllium from the beryllium concentrate to beryllium having the oxidation state 0. Furthermore, other metals, in particular aluminum and silicon, are reduced to the metals in oxidation states> 0. In order to prevent the possible reoxidation, the reaction can also be carried out in a substantially oxygen-free atmosphere. For example, protective gas, such as N ₂ , argon or a mixture thereof, is used for this purpose.

Preferably, the beryllium-containing (pre) alloy is an alloy which, in addition to beryllium, still the Metals aluminum and silicon (Al-Be-Si alloy) or aluminum, silicon, and another metal (Al-Be-M-Si alloy), wherein M is selected from the group consisting of chromium, nickel, copper or a mixture thereof.

Of Further, the inventive method to produce a beryllium-containing (pre) alloy another Step of cooling the reaction mixture after the step of reacting the solid mixture of starting materials takes place. In this Case is referred to in the sense of this invention of a master alloy, which contains considerable amounts of carbon and silicon in the alloy.

Accordingly, the present invention also relates to a (pre) alloy which can be obtained by the method according to the invention. An Al-Be-Si alloy thus obtained preferably has substantially the various components in the following proportions (mass%):
Al: 50 to 85, preferably 60 to 80, more preferably 70 to 75;
Be: 1 to 5, preferably 1.5 to 4.5, particularly preferably 2 to 4;
O: 2 × 10 ^-8 to 1 × 10 ^-5 ;
Si: 3 to 40, preferably 5 to 30, particularly preferably 10 to 25;
C: 0.5 to 5, preferably 1 to 4, particularly preferably 2 to 3;
with the proviso that the sum of all components should be 100.

An Al-Be-M-Si alloy thus obtained preferably has substantially the various components in the following proportions (% by mass):
Al: 2 to 15, preferably 3 to 12, particularly preferably 5 to 9;
Be: 1 to 5, preferably 1.5 to 4.5, particularly preferably 2 to 4;
M: 0 to 85, 55 to 80, more preferably 65 to 75;
O: 2 × 10 ^-8 to 1 × 10 ^-5 ;
Si: 5 to 35, preferably 7 to 30, particularly preferably 10 to 25;
C: 0.5 to 5, preferably 1 to 4, particularly preferably 2 to 3;
with the proviso that the sum of all components should be 100, where M is selected from the group consisting of chromium, nickel and copper.

Under "essentially have " here understood the fact that the (Vor) -Legierung a very small, therefore insignificant proportion of unavoidable impurities may contain.

A another embodiment The present invention also encompasses the use of the (pre) alloy for producing an alloy that is substantially free of oxygen is and has a carbon content of less than 0.5 mass is based on the total mass of the alloy. This can be done by one Producing and obtaining a (pre) alloy according to the above inventive method and then cooling down up to 1100 ° C and then Separation of oxygen and / or Carbon-containing compounds by the Seigerverfahren / filtration be accomplished. On the other hand, the separation of the oxygen and / or carbon-containing compounds by the Seigerverfahren / filtration also directly after the reaction of the solid mixture of starting materials without prior cooling to room temperature and Winning the (Vor) -Legierung done.

Under Segregation is understood in the sense of this invention segregation of Melting at the transition the melt in the solid / liquid Condition arise.

Therefore The present invention also relates to a process for the preparation a beryllium-containing alloy, in addition to the above-mentioned Step (s) the step of separating the segregation of the (pre) alloy according to the invention or Melt of the (pre) alloy comprises.

In the Seigerverfahren oxygen and / or carbon-containing compounds are removed, which have a higher melting point than the alloy of the invention and thus can be separated by filtration of the melt as a solid. In particular, the seiger process removes solid beryllium oxide and / or solid silicon carbide. In the case of addition of iron or iron oxide (Fe ₂ O ₃ , FeO or mixtures thereof) FeSi can also be removed. This is preferably true in the production of an Al-Be-Cu-Si alloy.

The segregation method is preferably most preferably at a temperature in the range of 590 to 1100 ° C, preferably in the range of 600 to 1000 ° C, more preferably in the range of 600 to 900 ° C in the range of 650 to 700 ° C performed.

The tapping of the master alloy after the reduction can be carried out batchwise or continuously in a pan, which is under protective gas. After cooling the melt (master alloy melt), the segregation products are preferably removed from the melt surface by cooling, or the melt is poured through a ceramic filter (Al ₂ O ₃ , SiC, quartz crack, etc.). The melt flows through the filter and the solid components remain on the surface.

Around To control the silicon content in the final alloy, the Master alloy directly before cooling corresponding amounts of carbon or iron are added. alternative can also be directly into the solid mixture of starting materials an appropriate amount of Fe oxide can be added. this has the advantage that silicon in the form of FeSi or SiC in the seiger process can be separated because these compounds have a higher melting point have as the produced beryllium-containing alloy.

Therefore The present invention also relates to an alloy obtained by the method according to the invention, that contains a seiger step, can be obtained.

An Al-Be-Si alloy thus obtained preferably has substantially the various components in the following proportions (mass%):
Al: 70 to 97, preferably 75 to 95, particularly preferably 80 to 93;
Be: 1.5 to 3.5, preferably 1.6 to 3, particularly preferably 1.7 to 2.5;
O: <2 × 10 ^-8 , preferably <1 × 10 ^-15 , more preferably <1 × 10 ^-25 ;
Si: 1 to 30, preferably 5 to 20, particularly preferably 10 to 18;
C: <0.5, preferably <0.5, more preferably 1 x 10 ^-3 , most preferably 1 x 10 ^-5 ;
with the proviso that the sum of all components should be 100.

An Al-Be-M-Si alloy thus obtained preferably has substantially the various components in the following proportions (% by mass):
Al: 4 to 12, preferably 6 to 11, particularly preferably 8 to 10;
Be: 2 to 5, preferably 2.5 to 4.5, particularly preferably 3 to 4;
M: 60 to 85, preferably 62 to 80, particularly preferably 64 to 75;
O: <2 × 10 ^-8 , preferably 1 × 10 ^-15 , particularly preferably 1 × 10 ^-18
Si: 1 to 30, preferably 5 to 28, particularly preferably 10 to 25;
C: <0.5, preferably 0.1, more preferably 1 x 10 ^-3 , most preferably 1 x 10 ^-5 ;
with the proviso that the sum of all components should be 100, where M is selected from the group consisting of chromium, nickel and copper.

In a preferred embodiment, the process of alloy production is as follows:
Be concentrate, reducing agent, metal compound and optionally iron oxide are added in the form of pellets or in the form of a mixture in an electric arc furnace, which is run under Ar overpressure. During reduction, the melt is tapped continuously or batchwise. The recovered alloy is tapped from the oven into a pan that is also under Ar overpressure. The alloy in the pan is cooled to an appropriate temperature and the solid phases formed are chamfered from the surface of the alloy or separated by filtration. As a filter, porous ceramic materials of Al ₂ O ₃ / SiC, quartz, etc. can be used.

Examples:

In all examples, 100 g Be concentrate with 92.34 g Be ₃ Al ₂ Si ₆ O ₁₈ and 8.1 g SiO ₂ was always used. Charcoal was used as the reducing agent. The metal components for the main alloying metals were used in metallic form (Cu, Al) or in oxidic form (Al ₂ O ₃ ).

Producing an Al-Be-Si master alloy

Example 1:

A batch containing 100 g of Be concentrate, 50 g of aluminum and 40 g of charcoal was reduced in an electric arc furnace. The batch was added in pellet form to the oven, operating under a slight argon overpressure. The reaction temperature was 2100 ° C. After the reduction wur the melt is poured into a BeO crucible, a sample taken and subjected to chemical analysis. The composition of the alloy was determined. Table 1 shows the amount, composition and beryllium yield of the resulting alloy.

Example 2:

The The same procedures as in Example 1 were carried out except that the temperature of the melting furnace was about 2200 ° C. In Table 1 are Amount, composition and beryllium yield of the resulting alloy specified.

Example 3:

It The same procedure was carried out as in Example 1 except that instead of 50 g of aluminum 100 g of aluminum was used. In table 1 is the amount, composition and beryllium yield of the obtained Alloy indicated.

Example 4:

The The same procedures as in Example 3 were carried out except that the temperature of the melting furnace was about 2200 ° C. In Table 1 are Amount, composition and beryllium yield of the resulting alloy specified.

Example 5:

It The same procedure was carried out as in Example 1 except that instead of 50 g of aluminum 150 g of aluminum was used. In table 1 is the amount, composition and beryllium yield of the obtained Alloy indicated.

Example 6:

The the same procedures as in Example 5 were carried out except that the temperature of the melting furnace was about 2200 ° C. In Table 1 are Amount, composition and beryllium yield of the resulting alloy specified.

Example 7:

It The same procedure was carried out as in Example 1 except that instead of 50 g of aluminum 200 g of aluminum was used. In table 1 is the amount, composition and beryllium yield of the obtained Alloy indicated.

Example 8:

The The same procedures as in Example 7 were carried out except that the temperature of the melting furnace was about 2200 ° C. In Table 1 are Amount, composition and beryllium yield of the resulting alloy specified.

Example 9:

It The same procedure was carried out as in Example 1 except that instead of 50 g of aluminum 250 g of aluminum was used. In table 1 is the amount, composition and beryllium yield of the obtained Alloy indicated.

Example 10:

The same procedure as in Example 9 was carried out except that the temperature of the melting furnace was about 2200 ° C. Table 1 shows the amount, composition and beryllium yield of the resulting alloy. Table 1: Wagon in [q] Temperature in [° C] alloy ore aluminum amorphous carbon Amount in [g] Al in [%] Be in [%] O in [%] Si in [%] C in [%] Yield in [%] Example 1 100 50 40 2100 53.94 67.7 2.15 1.33 28.1 2.04 27.75 Ex. 2 100 50 40 2200 76.25 55.65 4.48 1.92 37.44 2.44 76.25 Example 3 100 100 40 2100 125.23 70.6 2.28 1.3 25 2.16 61.6 Example 4 100 100 40 2200 121.99 70.6 3.1 1.7 25.5 2.56 81.5 Example 5 100 150 40 2100 164.75 76.7 2.2 1.4 19.07 2.02 78.4 Example 6 100 150 40 2200 166.68 76.2 2.4 1.8 18.93 2.44 85.7 Example 7 100 200 40 2100 212.61 81.1 2.05 1.5 14.9 1.88 93.76 Ex. 8 100 200 40 2200 212.57 80.8 1.93 1.9 14.96 2.29 88.46 Ex. 9 100 250 40 2100 259 84.2 1.7 1.5 12.3 1.78 94.84 Ex. 10 100 250 40 2200 2592 839 1.62 2 12.3 2.15 90.35

From Table 1 it can be seen that higher aluminum use increases the beryllium yield. In addition, the beryllium yield at 2100 ° C reaction temperature is higher than at 2200 ° C. It should also be noted that losses in yield are due to the formation of gaseous compounds. From the following Table 2 it can be seen that the beryllium or aluminum losses decrease by formation of gaseous compounds with increasing aluminum content in the starting composition and increase with the increase in temperature. Table 2: ° C used amount of aluminum 50 g 100 g 150 g 200 g 250 g Losses in [%] al Be al Be al Be al Be al Be 2100 31.54 6,118 19.13 6.8 16.86 6,659 15.5 6,244 14.06 5,157 2200 28.41 26.47 23.13 18.53 20.21 14.27 17.91 11.54 16,12 9,562

Example 11:

A batch containing 100 g of Be concentrate, 300 g of Al ₂ O ₃ and 131 g of charcoal was reduced in an electric arc furnace.

there The batch was pelletized in the oven under an Ar overpressure is driven, added. The reduction temperature was 2100 ° C. After Reduction, the melt was poured into a BeO crucible and a Taken sample, which was subjected to chemical analysis. The Composition of the alloy became specific. In Table 3 are Amount and composition of the resulting alloy indicated.

Example 12:

The the same procedures as in Example 11 were carried out except that the temperature of the melting furnace was about 2150 ° C.

In Table 3 is the amount and composition of the resulting alloy specified.

Example 13:

The the same procedures as in Example 11 were carried out except that the temperature of the melting furnace was about 2200 ° C.

In Table 3 is the amount and composition of the resulting alloy specified.

Examples 14 to 16:

In Examples 14 to 16, the same procedure as in Examples 11 to 13 was carried out except that 350 g of Al ₂ O ₃ and 151 g of charcoal were used. Table 3 shows the amount and composition of the alloy obtained.

Examples 17 to 19:

In Examples 17 to 19, the same procedure as in Examples 11 to 13 was carried out except that 400 g of Al ₂ O ₃ and 165 g of charcoal were used. Table 3 shows the amount and composition of the alloy obtained.

Examples 20 to 22:

In Examples 20 to 22, the same procedure as in Examples 11 to 13 was carried out except that 500 g of Al ₂ O ₃ and 180 g of charcoal were used. Table 3 shows the amount and composition of the alloy obtained. Table 3: ° C Alloy mass [g] Alloy composition [%] BeO (fixed) [g] al Be O Si C Example 11 2100 113.49 71.85 2.1393 1.38 24,02 1.9912 3.0499 Example 12 2150 100.93 69.943 2.6611 1.85 25.54 1.8559 0 Example 13 2200 89.76 68.282 2.4114 2.18 27.419 1.8877 0 Example 14 2100 121.72 73.329 2.2876 1.32 22.251 2.1321 1.4576 Example 15 2150 125.53 73.299 2.2443 1.45 21.992 2.4652 0 Example 16 2200 112.01 71.625 2.0534 1.71 23.809 2.5123 0 Example 17 2100 131.59 75.159 2.2436 1.36 20.528 2.0687 8.6092 Example 18 2150 130.62 74.811 2,103 1.53 20.779 2.3076 0 Example 19 2200 115.21 73.105 1.92 1.81 22.629 2.3456 0 Example 20 2100 114.61 76.286 1.6065 0,018 20.716 1.3911 4.3022 Example 21 2150 94.998 74.109 2.2633 0.024 22.324 1.3033 0 Example 22 2200 77.355 72.251 2.0035 0,029 24.435 1.3107 0

Table 3 shows that the complete beryllium reduction takes place only at temperatures above 2100 ° C. In addition, at temperatures above 2150 ° C, the alloy yields decrease. The highest metal yields are achieved at a reaction temperature of 2150 ° C, all temperatures shown are acceptable according to the invention. The experiments also show that higher Al ₂ O ₃ content, reduce the amount of recoverable alloy.

Seigerverfahren

Example 23:

First, the alloy melt obtained in Example 9 was poured through a Al ₂ O ₃ filter at a temperature of 650 ° C. In this case, the amounts of solids of Al ₄ C ₄ Si, SiC and BeO stated in Table 5 were separated off. Subsequently, the melt was allowed to cool to room temperature. The alloy was chemically analyzed and the filter residue deposited on the filter was X-ray examined. The amount and composition of the recovered alloy are shown in Table 4.

Example 24:

First, the procedure carried out in Example 9 was applied analogously, with the difference that the melt was subjected to a seiger process at a temperature of 700 ° C. Here, the melt was poured through an Al ₂ O ₃ filter to separate the segregations in the form of solids. In this case, the amounts of solid stated in Table 5 were separated off from Al ₄ C ₄ Si and BeO. Subsequently, the melt was allowed to cool to room temperature. The alloy was chemically analyzed and the filter residue deposited on the filter was X-ray examined. The amount and composition of the recovered alloy are shown in Table 4. It can also be seen that at A temperature of about 650 ° C SiC is no longer separable as a solid, which increases the proportion of Si in the alloy and thus somewhat reduces their quality. Table 4: Seigert temperature [° C] Quantity [g] Composition of the alloy [%] al Be O Si C Example 23 650 ° C 241.9 86.97 1,821 0.65 × 10 ^-26 11.2 0.68 × 10 ^-7 Example 24 700 ° C 241.56 86.45 1,824 0.414 × 10 ^-26 11.7 0.24 × 10 ^-6 Table 5: Seigert temperature [° C] Solids [g] Al ₄ C ₄ Si SiC BOe Example 21 650 ° C 21.235 2.29 0.625 × 10 ^-6 Example 22 700 ° C 23.866 0 0.625 × 10 ^-6

Example 25:

First, the melt of Example 18 was subjected to the Seiger process at a temperature of 700 ° C. Here, the melt was poured through an Al ₂ O ₃ filter to separate the segregations in the form of solids. In this case, the amounts of solids of SiC and BeO indicated in Table 7 were separated off. Subsequently, the melt was allowed to cool to room temperature. The alloy was chemically analyzed and the filter residue deposited on the filter was X-ray examined. The amount and composition of the recovered alloy are shown in Table 6.

Example 26:

First, the melt of Example 18 was subjected to the Seiger process at a temperature of 600 ° C. Here, the melt was poured through an Al ₂ O ₃ filter to separate the segregations in the form of solids. In this case, the amounts of solid Si, SiC and BeO indicated in Table 7 were separated off. Subsequently, the melt was allowed to cool to room temperature. The alloy was chemically analyzed and the filter residue deposited on the filter was X-ray examined. The amount and composition of the recovered alloy are shown in Table 6.

Example 27:

First, the melt was cooled to a temperature of 580 ° C. Here, the melt was mostly solidified, so that the segregation step was no longer possible. Table 6: Seigert temperature [° C] Quantity [g] Composition of the alloy [%] al Be O Si C Example 25 700 120.56 81.06 2,279 3.03 × 10 ^-27 16.567 1.53 × 10 ^-7 Example 26 600 116.15 84.13 2,365 4.67 × 10 ^-31 13,504 7.76 × 10 ^-8 Table 7: Seigert temperature [° C] filtered-off solids [g] Si SiC BeO Example 25 700 0 10.062 3.13 × 10 ^-7 Example 26 600 4.407 10.062 3.13 × 10 ^-7

As from Table 6 from the composition and from Table 7 of the When Si separated out in Example 26 is apparent, it is at a seiger temperature of 600 ° C possible, Partial Si to be partially separated. This gives an alloy with a lower silicon content than at a seiger temperature of over 600 ° C.

Preparation of an Al-Be-Cu-Si alloy

Example 28:

It was a batch containing 100 g Be concentrate, 75 g copper and 40 g Charcoal contained, reduced in an electric arc furnace.

The batch in pelet form was added to the oven, which was run under a small Ar overpressure. The reduction temperature was 2200 ° C. After reduction, the melt was cast at a temperature of 1000 ° C through an Al ₂ O ₃ filter. In this way, the solids given in Table 9 were separated in the stated amount.

The Composition was subjected to chemical analysis.

The Composition of the alloy is given in Table 8.

Example 29:

The same procedure was carried out as given in Example 28, except that the Seiger process was carried out at 800 ° C. In this way, the solids given in Table 9 were separated in the stated amount. The composition of the alloy is shown in Table 8. Table 8: Seigert temperature [° C] Quantity [g] Composition of the alloy [%] al Be Cu O Si C Example 28 1000 105.124 7.7022 3.7299 65.282 0.45674 × 10 ^-14 23 285 0.04027 × 10 ^-6 Example 29 800 88.855 9.1124 3,034 73.733 0,43946 × 10 ^-24 13,504 0,23395 × 10 ^-8 Table 9: Seigert temperature [° C] filtered-off solids [g] SiC Si BeO Example 28 1000 0.70445 0.50148 0.405 × 10 ^-6 Example 29 800 0.70446 12.4332 3 × 10 ^-9

Example 30:

The same procedure as in Example 28 was carried out eight times (Examples 30 a) to h)), respectively but with the difference that instead of 75 g of copper 175 g of copper were used. In Examples 30 b) to h), the amounts of iron indicated in Table 10 were added at the end of the reduction at the reduction temperature. Small differences are also to be taken from Table 10 with respect to the Seigertemperatur. Table 10: Reduction temperature in ° C Seigertem temperature in ° C Amount of Fe in g Amount of Al in g Quantity Be in g Amount of Cu in g Amount of Si in g Amount of Fe in g Quantity O in g Quantity C in g Example 30 a) 2200 none 0 4.26 2.11 78.73 14.46 0.35 9.00 × 10 ^-08 0.74 Ex. 30 b) 2200 1100 0 4.42 2.19 81.22 12.14 1,00E ^-02 5.00 × 10 ^-20 2.10 × 10 ^-07 Example 30 c) 2200 1000 10 4.53 2.24 83.33 9.87 0.01 5.00 × 10 ^-20 3,00 × 10 ^-07 Example 30 d) 2200 1000 20 4.65 2.3 85.54 7.47 0.01 5.00 × 10 ^-20 4.70 × 10 ^-07 Ex. 30 e) 2200 1100 28 4.94 2.45 91.28 0.73 0.59 8.00 × 10 ^-18 4.00 × 10 ^-05 Example 30 f) 2200 1000 30 4.78 2.37 87.87 4.95 0.02 6.00 × 10 ^-20 1.00 × 10 ^-06 Ex. 30 g) 2200 1000 48 4.99 2.33 91.75 0.46 0.45 1.00 × 10 ^-19 7.00 10 ^-06 Eg 30 h) 2200 1100 48 4.96 2.46 91.21 0.61 0.75 9.00 × 10 ^-18 4.00 × 10 ^-05

As From Table 10, the Si content of the alloy be adjusted by the Fe addition before the segregation targeted.

Example 31:

The same procedure was carried out as in Example 28, with the difference that instead of 75 g of copper 175 g of copper and instead of 40 g of charcoal 60 g of charcoal were used. In addition, 80 g of Fe ₂ O _{3 were} initially added to the batch. Subsequently, the seiger process was carried out as in Example 28, but at a temperature of 1100 ° C. The composition of the alloy thus obtained is given in Table 11. Table 11: Al in g Be in g Cu in g S in g Fe in g O in g C in g Before alloy melt 3.97 1.93 69,83 9.35 14.76 7.00 × 10 ^-08 0.15 at 2200 ° C After segregation at 1100 ° C 5.17 2.52 90.99 0.72 0.59 8.00 × 10 ^-18 4.00 × 10 ^-05

By the addition of iron to the master alloy melt and the addition of Fe ₂ O ₃ to the initial charge, Si is purged in the Seiger process in the form of a high-melting compound (FeSi).

Claims (19)

Process for the preparation of a beryllium-containing (Before) alloy, which includes the following step: Reacting a solid mixture of starting materials at a temperature that is sufficient to form a beryllium-containing alloy, wherein the solid mixture Starting materials include a beryllium concentrate and a metal component includes. Method according to claim 1, wherein the reaction is at a temperature in the range of 1700 up to 2500 ° C he follows. Method according to claim 1 or 2 wherein the metal component is selected from the group consisting of which consists of the following: Metals selected from the group made of aluminum, chromium, nickel, copper and a mixture thereof consists; Carbonates of metals selected from the group which consists of nickel, copper and a mixture thereof; Oxide the metals selected from the group consisting of aluminum, Chromium, nickel, copper and a mixture thereof, and mixtures from that. Method according to one the claims 1 to 3, wherein the mass ratio of beryllium concentrate to metal in the metal component in the range from 3/1 to 1/5. Method according to one the claims 1 to 4, wherein the beryllium concentrate is the ore beryl. Method according to one the claims 1 to 5, wherein the reaction in the presence of a reducing agent carried out becomes. Method according to claim 6, wherein the reducing agent is charcoal. Method according to claim 7, wherein the mass ratio Charcoal to the ore beryl ranges from 3/10 to 3/1. Method according to one the claims 5 to 8, wherein the reducing agent serves beryllium from the To reduce ore to beryllium with the oxidation state 0. Method according to one the claims 1 to 9, wherein the beryllium-containing alloy is an Al-Be-Si alloy or an Al-Be-M-Si alloy, where M is selected from the group which consists of chromium, nickel, copper or a mixture thereof. Method according to one the claims 1 to 10, which is the further step of cooling the reaction product comprising, after the step of reacting the solid mixture of starting materials. (Vor) -Legierung, by a procedure after a the claims 1 to 11 available is. (Pre) alloy having substantially the following composition (I) or (II): Composition (I): al: 50 to 85 mass% Be: 1 to 5 mass% O: 2 × 10 ^-8 to 1 × 10 ^-5 mass% Si: 3 to 40 mass% C: 0.5 to 5 mass% Composition (II): al: 2 to 15 mass% Be: 1 to 5 mass% M: 50 to 85 mass% O: 2 × 10 ^-8 to 1 × 10 ^-5 mass% Si: 5 to 35 mass% C: 0.5 to 5 Mass% with the proviso that the sum of all alloy components is 100, where M is selected from the group consisting of chromium, nickel and copper. Use of the (pre) alloy according to claim 12 or 13 for producing an alloy that is substantially free is of oxygen and has a carbon content that is smaller is 0.5 mass%, based on the total mass of the alloy. Process for the preparation of a beryllium-containing An alloy comprising the step of: seeding a (pre) alloy according to claim 12 or 13. Method according to claim 15, wherein the segregation by solid beryllium oxide and / or solid Silicon carbide is / will be removed. Method according to claim 15 or 16, the segregation being at a temperature in the range from 500 to 1100 ° C (preferably 600 to 1000 ° C) carried out becomes. Alloy obtained by a method according to one of claims 15 to 17 available is. Alloy having substantially the following composition (III) or (IV): Composition (III): al: 70 to 97 mass% Be: 1.5 to 3.5 mass% O: <2 × 10 ^-8 mass% Si: 1 to 30 mass% C: <0.5 mass% Composition (IV): al: 4 to 12 mass% Be: 2 to 5 mass% M: 60 to 85 mass% O: <2 × 10 ^-8 mass% Si: 1 to 30 mass% C: <0.5 Mass% with the proviso that the sum of all alloy components is 100, where M is selected from the group consisting of chromium, nickel and copper.