CN103966512A - Large-size gradient-aluminum-content iron-chromium-aluminum ODS (oxide dispersion strengthened) alloy sheet material, and preparation method and application thereof - Google Patents
Large-size gradient-aluminum-content iron-chromium-aluminum ODS (oxide dispersion strengthened) alloy sheet material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a large-size gradient-aluminum-content iron-chromium-aluminum ODS (oxide dispersion strengthened) alloy sheet material, and a preparation method and application thereof, and aims to solve the problem of incapability of compromising oxidation resistance and weldability in the existing thermal protection system metal cellular-structure veneer sheet. The thickness of the material is 10-300 mu m, and the diameter is 1000mm; one side of the sheet is composed of Cr, Al, Y2O3 and the balance of Fe; and the other side is composed of Cr, Al, Y2O3 and the balance of Fe. The method comprises the following steps: putting an aluminiferous ingot into a water-cooled copper crucible, putting a yttrium oxide ceramic column or yttrium oxide powder into another water-cooled copper crucible, heating a high-temperature alloy substrate to 650-1000 DEG C, and keeping the temperature; and evaporating the aluminiferous ingot and yttrium oxide ceramic ingot or yttrium oxide powder, and naturally cooling to 50 DEG C. The material has favorable oxidation resistance, one side is oxidation-resistant, and the other side is easy for welding. The method belongs to the field of preparation of a metal cellular-structure upper/lower veneer sheet material for a thermal protection system.
Description
Technical field
The present invention relates to a kind of thin plate material and its preparation method and application.
Background technology
Spacecraft surface in atmospheric reentry process produces high temperature with air friction, and is subject to small aerolite, the hypervelocity impact of space debris, and the corrosion of near-earth atmospheric layer rainwater etc. test.Thermal protection system can reduce the heat that enters spacecraft inside as far as possible, and spacecraft body and internal part are worked within the scope of reasonable temperature, is therefore the important component part of spacecraft.Patent " for the metal honeycomb structure of thermal protection system and the cover plate of Ceramic bond " (patent No. 101791880B) has proposed a kind of metal alloy cover board that comprises honeycomb, top plate, lower plywood, phase change material, shell and ceramic plate, for thermal protection system.Compared with ceramic insulation tile, it is high that metal honeycomb structure has reliability, good toughness, and the advantage such as do not absorb water.Wherein the material of honeycomb, top plate and lower plywood is Ni based high-temperature alloy, Fe based high-temperature alloy, Ni-Fe based high-temperature alloy, Co based high-temperature alloy or Nb based high-temperature alloy, and the mode of connection of honeycomb and top plate, lower plywood is high temperature vacuum brazing.Fe base ODS alloy still has very high hot strength, high temperature creep property and antioxidant property near approaching fusing point, especially the ferrum-chromium-aluminum ODS alloy of high aluminium content, because high-temperature oxidation resistance is good, can significantly improve the use temperature of material, therefore be suitable for the laminate up and down of thermal protection system metal honeycomb structure.But the ferrum-chromium-aluminum ODS alloy of high aluminium content cannot be with honeycomb by being welded to connect because aluminium content is high.
Summary of the invention
The object of the invention is the problem that can take into account in order to solve existing thermal protection system metal honeycomb structure laminate antioxidant property and weldability, a kind of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material, preparation method and application are provided.
Large size gradient aluminium content ferrum-chromium-aluminum ODS latten material thickness is 10-300um, and diameter is 1000mm, thin plate one side by weight percentage composition by 15.0%-40.0%Cr, 10.0%-30.0%Al, 0.3%-0.6%Y
2o
3and the Fe of equal amount composition, opposite side by weight percentage composition by 15.0%-40.0%Cr, 0%-5.0%Al, 0.3%-0.6%Y
2o
3and the Fe of equal amount composition.
The preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material carries out according to following steps:
One, will put into water jacketed copper crucible containing aluminium ingot material, placing 35 grams of tungsten containing in aluminium ingot surface, yttrium post or yttrium oxide powder are put into another water jacketed copper crucible, in yttrium oxide ingot surface, place 10-15 gram of Calcium Fluoride (Fluorspan), high-temperature alloy base sheet is installed on frame substrate, use dehydrated alcohol wipe surfaces, be evacuated to 1 × 10
-3pa-5 × 10
-3pa, is then heated to 650-1000 DEG C by superalloy substrate, insulation;
Two, adopt baffle plate to block the superalloy substrate through step 1 processing, two electron beam currents are increased to respectively to 1.6-3A and 1.0-1.5A, and stable 1-20min, open baffle plate, on superalloy substrate, deposit thickness is the CaF of 1-10 μ m
2;
Three, adopting the evaporation of 1.6-3A electron beam current containing aluminium ingot material 10-60min, adopt 1.0-1.5A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 10-60min, is 1 × 10 in vacuum tightness
-3pa-5 × 10
-3under the condition of Pa, naturally cool to 50 DEG C, obtain large size gradient aluminium content ferrum-chromium-aluminum ODS latten material;
Described in step 1, be one or both in FeCrAl-Al sandwich ingot, FeCrAl alloy ingot and fine aluminium ingot containing aluminium ingot material, described FeCrAl-Al sandwich ingot is inserted in FeCrAl alloy or FeCr alloy and is formed by fine aluminium bar.
Described large size gradient aluminium content ferrum-chromium-aluminum ODS latten material, as top plate and lower plywood, is applied to thermal protection system metal honeycomb structure, and low aluminium one side is connected by high temperature brazing technique with honeycomb.
The present invention is directed to the preparation method that the application background of the upper and lower laminate of metal honeycomb structure proposes a kind of ultra-thin, large size, easily welds anti-oxidant gradient aluminium content ferrum-chromium-aluminum ODS latten material, than the iron-base superalloy thin plate material thin thickness of existing same size, iron-base superalloy thin plate material size than existing same thickness is large, antioxidant property than the iron-base superalloy thin plate material of existing similar sizes and thickness is good, and it is anti-oxidant to have a side, opposite side is easy to the feature of welding.
The present invention has the following advantages:
(1) the prepared ferrum-chromium-aluminum ODS latten material thickness thin (10-300um) of the inventive method, is easy to realize the object of lightweight;
(2) the prepared ferrum-chromium-aluminum ODS latten scantling of the inventive method large (diameter 1000mm), is convenient to cut out and is processed into needed geomery;
(3) the prepared ferrum-chromium-aluminum ODS latten material high alumina one side aluminium content high (10.0wt.%-30.0wt.%) of the inventive method, antioxidant property is good, and (in 1100 DEG C of 100h air, oxidation weight gain is not higher than 0.8mg/cm
2);
(4) prepared low aluminium one side of ferrum-chromium-aluminum ODS latten material of the inventive method is easily welded;
(5) the inventive method process costs is low, and without carrying out complicated high temperature rolling, technique is simple.
In sum, ferrum-chromium-aluminum ODS latten material involved in the present invention and preparation method thereof is applicable to being applied to the metal honeycomb structure levels panel material of thermal protection system.
Brief description of the drawings
Fig. 1 is the schematic diagram of FeCrAl-Al sandwich ingot in experiment one step 1, and in figure, 1 represents fine aluminium bar, and 2 represent FeCrAl alloy;
Fig. 2 tests one to the projected position schematic diagram of testing water jacketed copper crucible used in three, and in figure, 1,3 represent diameter 68.5mm water jacketed copper crucibles, and 2,4 represent diameter 98.5mm water jacketed copper crucibles;
Fig. 3 is that experiment one is to testing the position view of the three large size gradient aluminium content ferrum-chromium-aluminum ODS latten materials of preparing in thermal protection system metal honeycomb structure, in figure, 4 represent thermal protection system metal honeycomb structure top plate, 5 represent thermal protection system metal honeycomb structure honeycomb, and 6 represent thermal protection system metal honeycomb structure lower plywood.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment large size gradient aluminium content ferrum-chromium-aluminum ODS latten material thickness is 10-300um, diameter is 1000mm, thin plate one side by weight percentage composition by 15.0%-40.0%Cr, 10.0%-30.0%Al, 0.3%-0.6%Y
2o
3and the Fe of equal amount composition, opposite side by weight percentage composition by 15.0%-40.0%Cr, 0%-5.0%Al, 0.3%-0.6%Y
2o
3and the Fe of equal amount composition.
Embodiment two: described in embodiment one, the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material carries out according to following steps:
One, will put into water jacketed copper crucible containing aluminium ingot material, placing 35 grams of tungsten containing in aluminium ingot surface, yttrium post or yttrium oxide powder are put into another water jacketed copper crucible, in yttrium oxide ingot surface, place 10-15 gram of Calcium Fluoride (Fluorspan), high-temperature alloy base sheet is installed on frame substrate, use dehydrated alcohol wipe surfaces, be evacuated to 1 × 10
-3pa-5 × 10
-3pa, is then heated to 650-1000 DEG C by superalloy substrate, insulation;
Two, adopt baffle plate to block the superalloy substrate through step 1 processing, two electron beam currents are increased to respectively to 1.6-3A and 1.0-1.5A, and stable 1-20min, open baffle plate, on superalloy substrate, deposit thickness is the CaF of 1-10 μ m
2;
Three, adopting the evaporation of 1.6-3A electron beam current containing aluminium ingot material 10-60min, adopt 1.0-1.5A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 10-60min, is 1 × 10 in vacuum tightness
-3pa-5 × 10
-3under the condition of Pa, naturally cool to 50 DEG C, obtain large size gradient aluminium content ferrum-chromium-aluminum ODS latten material;
Described in step 1, be one or both in FeCrAl-Al sandwich ingot, FeCrAl alloy ingot and fine aluminium ingot containing aluminium ingot material, described FeCrAl-Al sandwich ingot is inserted in FeCrAl alloy or FeCr alloy and is formed by fine aluminium bar.
Described FeCrAl-Al sandwich ingot is by diameter 19mm-25mm, and the fine aluminium bar of height 200mm-300mm inserts diameter 98.5mm, composition in the FeCrAl alloy of height 200mm-300mm or FeCr alloy.
The aluminium ingot material that contains described in present embodiment step 1 is put into water jacketed copper crucible before first at 200 DEG C of placement 4h.
Embodiment three: what present embodiment was different from embodiment two is to be evacuated to 3 × 10 in step 1
-3pa.Other is identical with embodiment two.
Embodiment four: what present embodiment was different from embodiment two or three is, in step 1, superalloy substrate is heated to 660 DEG C, insulation.Other is identical with embodiment two or three.
Embodiment five: what present embodiment was different from one of embodiment two to four is to adopt the evaporation of 2A electron beam current containing aluminium ingot material 20min in step 3.Other is identical with one of embodiment two to four.
Embodiment six: what present embodiment was different from one of embodiment two to five is to adopt the evaporation of 2.5A electron beam current containing aluminium ingot material 40min in step 3.Other is identical with one of embodiment two to five.
Embodiment seven: what present embodiment was different from one of embodiment two to six is to adopt 1.2A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 30min in step 3.Other is identical with one of embodiment two to six.
Embodiment eight: what present embodiment was different from one of embodiment two to seven is to adopt 1A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 40min in step 3.Other is identical with one of embodiment two to seven.
Embodiment nine: the large size gradient aluminium content ferrum-chromium-aluminum ODS latten material described in one of embodiment one to eight is as top plate and lower plywood, be applied to thermal protection system metal honeycomb structure, low aluminium one side is connected by high temperature brazing technique with honeycomb.
Adopt following experimental verification effect of the present invention:
Experiment one:
The preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material carries out according to following steps:
One, the FeCrAl-Al sandwich ingot of diameter 98.5mm is put into water jacketed copper crucible 2, in FeCrAl-Al sandwich ingot surface, place 35 grams of tungsten, yttrium post is put into another water jacketed copper crucible 1, on yttrium post, place 10-15 gram of Calcium Fluoride (Fluorspan), high-temperature alloy base sheet is installed on frame substrate, use dehydrated alcohol wipe surfaces, be evacuated to 2 × 10
-3pa, is then heated to 660 DEG C by superalloy substrate, insulation;
Two, adopt baffle plate to block the superalloy substrate through step 1 processing, two electron beam currents are increased to respectively to 2.8A and 1.3A, and stable 1-20min (occurring obvious molten bath to ingot surface), open baffle plate, on superalloy substrate, deposit thickness is the CaF of 1-10 μ m
2;
Three, under the condition that is 550mm at target-substrate distance, adopting 2.8A electron beam current evaporation FeCrAl-Al sandwich ingot 20min, adopt 1.3A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 30min, is 3 × 10 in vacuum tightness
-3under the condition of Pa, naturally cool to 50 DEG C, obtain large size gradient aluminium content ferrum-chromium-aluminum ODS latten material;
In the FeCrAl alloy of the sandwich of FeCrAl-Al described in step 1 ingot by fine aluminium bar insertion diameter 98.5mm, the height 200mm-300mm of diameter 19mm-25mm, height 200mm-300mm, form.
The diameter of the substrate of superalloy described in step 1 is 1000mm.
The large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation can be used for preparing thermal protection system metal honeycomb structure (seeing Fig. 3), in Fig. 3,4 represent thermal protection system metal honeycomb structure top plate, 5 represent thermal protection system metal honeycomb structure honeycomb, 6 represent thermal protection system metal honeycomb structure lower plywood, the large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation is as in thermal protection system metal honeycomb structure top plate high alumina one side direction, under low aluminium one side direction, be connected by high temperature vacuum brazing technique with the metal honeycomb structure of thermal protection system shown in 5 honeycomb, the large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation is as in low aluminium one side direction of thermal protection system metal honeycomb structure lower plywood, be connected by high temperature vacuum brazing technique with the metal honeycomb structure of thermal protection system shown in 5 honeycomb, under high alumina one side direction.
Experiment two:
The preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material carries out according to following steps:
One, the FeCrAl alloy ingot of diameter 98.5mm is put into water jacketed copper crucible 2, in FeCrAl alloy ingot surface, place Calcium Fluoride (Fluorspan), the fine aluminium ingot of diameter 68.5mm is put into another water jacketed copper crucible 1 after drying, yttrium post is put into water jacketed copper crucible 3, high-temperature alloy base sheet is installed on frame substrate, use dehydrated alcohol wipe surfaces, be evacuated to 4 × 10
-3pa, is then heated to 800 DEG C by superalloy substrate, insulation;
Two, adopt baffle plate to block the superalloy substrate through step 1 processing, two electron beam currents are increased to respectively to 2.5A and 1.5A, and stable 1-20min (occurring obvious molten bath to ingot surface), open baffle plate, on superalloy substrate, deposit thickness is the CaF of 1-10 μ m
2;
Three, under the condition that is 550mm at target-substrate distance, adopt 2.5A electron beam current evaporation FeCrAl alloy ingot 50min, adopting 1.5A electron beam current evaporation oxidation yttrium pottery ingot 50min, adopt 1.5A electron beam current evaporation fine aluminium ingot 25min, is 3 × 10 in vacuum tightness
-3under the condition of Pa, naturally cool to 50 DEG C, obtain large size gradient aluminium content ferrum-chromium-aluminum ODS latten material;
The diameter of the substrate of superalloy described in step 1 is 1000mm.
The large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation can be used for preparing thermal protection system metal honeycomb structure (seeing Fig. 3), in Fig. 3,4 represent thermal protection system metal honeycomb structure top plate, 5 represent thermal protection system metal honeycomb structure honeycomb, 6 represent thermal protection system metal honeycomb structure lower plywood, the large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation is as in thermal protection system metal honeycomb structure top plate high alumina one side direction, under low aluminium one side direction, be connected by high temperature vacuum brazing technique with the metal honeycomb structure of thermal protection system shown in 5 honeycomb, the large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation is as in low aluminium one side direction of thermal protection system metal honeycomb structure lower plywood, be connected by high temperature vacuum brazing technique with the metal honeycomb structure of thermal protection system shown in 5 honeycomb, under high alumina one side direction.
Experiment three:
The preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material carries out according to following steps:
One, the FeCrAl alloy ingot of two diameter 98.5mm is put into respectively to water jacketed copper crucible 2 and water jacketed copper crucible 4, in FeCrAl alloy ingot surface, place Calcium Fluoride (Fluorspan), the fine aluminium ingot of diameter 68.5mm is put into another water jacketed copper crucible 1 after drying, yttrium post is put into water jacketed copper crucible 3, high-temperature alloy base sheet is installed on frame substrate, use dehydrated alcohol wipe surfaces, be evacuated to 2 × 10
-3pa, is then heated to 900 DEG C by superalloy substrate, insulation;
Two, adopt baffle plate to block the superalloy substrate through step 1 processing, two electron beam currents are increased to respectively to 3A and 1.5A, and stable 1-20min, open baffle plate, on superalloy substrate, deposit thickness is the CaF of 1-10 μ m
2;
Three, under the condition that is 550mm at target-substrate distance, adopt 3A electron beam current evaporation FeCrAl alloy ingot 60min, adopting 1.5A electron beam current evaporation oxidation yttrium pottery ingot 60min, adopt 1.5A electron beam current evaporation fine aluminium ingot 30min, is 2 × 10 in vacuum tightness
-3under the condition of Pa, naturally cool to 50 DEG C, obtain large size gradient aluminium content ferrum-chromium-aluminum ODS latten material;
The diameter of the substrate of superalloy described in step 1 is 1000mm.
The large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation be can be used for preparing thermal protection system metal honeycomb structure (seeing Fig. 3), in Fig. 3,4 represent thermal protection system metal honeycomb structure top plate, 5 represent thermal protection system metal honeycomb structure honeycomb, 6 represent thermal protection system metal honeycomb structure lower plywood, the large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation is as in thermal protection system metal honeycomb structure top plate high alumina one side direction, under low aluminium one side direction, be connected by high temperature vacuum brazing technique with the metal honeycomb structure of thermal protection system shown in 5 honeycomb, the large size gradient aluminium content ferrum-chromium-aluminum ODS latten material of this experiment preparation is as in low aluminium one side direction of thermal protection system metal honeycomb structure lower plywood, be connected by high temperature vacuum brazing technique with the metal honeycomb structure of thermal protection system shown in 5 honeycomb, under high alumina one side direction.
Claims (9)
1. large size gradient aluminium content ferrum-chromium-aluminum ODS latten material, it is characterized in that described large size gradient aluminium content ferrum-chromium-aluminum ODS latten material thickness is 10-300um, diameter is 1000mm, thin plate one side by weight percentage composition by 15.0%-40.0%Cr, 10.0%-30.0%Al, 0.3%-0.6%Y
2o
3and the Fe of equal amount composition, opposite side by weight percentage composition by 15.0%-40.0%Cr, 0%-5.0%Al, 0.3%-0.6%Y
2o
3and the Fe of equal amount composition.
2. the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material described in claim 1, is characterized in that the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material carries out according to following steps:
One, will put into water jacketed copper crucible containing aluminium ingot material, placing 35 grams of tungsten containing in aluminium ingot surface, yttrium post or yttrium oxide powder are put into another water jacketed copper crucible, in yttrium oxide ingot surface, place 10-15 gram of Calcium Fluoride (Fluorspan), high-temperature alloy base sheet is installed on frame substrate, use dehydrated alcohol wipe surfaces, be evacuated to 1 × 10
-3pa-5 × 10
-3pa, is then heated to 650-1000 DEG C by superalloy substrate, insulation;
Two, adopt baffle plate to block the superalloy substrate through step 1 processing, two electron beam currents are increased to respectively to 1.6-3A and 1.0-1.5A, and stable 1-20min, open baffle plate, on superalloy substrate, deposit thickness is the CaF of 1-10 μ m
2;
Three, adopting the evaporation of 1.6-3A electron beam current containing aluminium ingot material 10-60min, adopt 1.0-1.5A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 10-60min, is 1 × 10 in vacuum tightness
-3pa-5 × 10
-3under the condition of Pa, naturally cool to 50 DEG C, obtain large size gradient aluminium content ferrum-chromium-aluminum ODS latten material;
Described in step 1, be one or both in FeCrAl-Al sandwich ingot, FeCrAl alloy ingot and fine aluminium ingot containing aluminium ingot material, described FeCrAl-Al sandwich ingot is inserted in FeCrAl alloy or FeCr alloy and is formed by fine aluminium bar.
3. the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material according to claim 2, is characterized in that being evacuated to 3 × 10 in step 1
-3pa.
4. the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material according to claim 2, is characterized in that, in step 1, superalloy substrate is heated to 660 DEG C, insulation.
5. the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material according to claim 2, is characterized in that adopting the evaporation of 2A electron beam current containing aluminium ingot material 20min in step 3.
6. the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material according to claim 2, is characterized in that adopting the evaporation of 2.5A electron beam current containing aluminium ingot material 40min in step 3.
7. the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material according to claim 2, is characterized in that adopting in step 3 1.2A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 30min.
8. the preparation method of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material according to claim 2, is characterized in that adopting in step 3 1A electron beam current evaporation oxidation yttrium pottery ingot or yttrium oxide powder 40min.
9. the application of large size gradient aluminium content ferrum-chromium-aluminum ODS latten material described in claim 1, is characterized in that described large size gradient aluminium content ferrum-chromium-aluminum ODS latten material, as top plate and lower plywood, is applied to thermal protection system metal honeycomb structure.
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| CN105909700B (en) * | 2015-02-23 | 2019-03-26 | 株式会社岛野 | Anti-corrosion bicycle disk brake rotor |
| CN114959561A (en) * | 2022-06-29 | 2022-08-30 | 中国航发动力股份有限公司 | MCrAlX bonding layer with gradient change of Al content and preparation method thereof |
| CN114959561B (en) * | 2022-06-29 | 2024-02-27 | 中国航发动力股份有限公司 | MCrAlX bonding layer with gradient Al content change and preparation method thereof |
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