CN103966512B - Large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material, preparation method and application - Google Patents
Large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material, preparation method and application Download PDFInfo
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Abstract
The preparation method of large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material, the present invention is the problem that can take into account in order to solve existing thermal protection system metal honeycomb structure laminate antioxygenic property and weldability. Method is as follows: will put into water jacketed copper crucible containing aluminium ingot material, yttrium post or yittrium oxide powder are put into another water jacketed copper crucible, high temperature alloy substrate is heated to 650-1000 DEG C, insulation; Evaporation contains aluminium ingot material and yttrium ingot or yittrium oxide powder and naturally cools to 50 DEG C, to obtain final product. The antioxygenic property of material of the present invention is good, and a side is anti-oxidant, and opposite side is easy to welding. The invention belongs to the preparation field of the metal honeycomb structure levels plate material of thermal protection system.
Description
Technical field
The present invention relates to a kind of preparation method of light sheet material.
Background technology
Spacecraft surface in atmospheric reentry process produces high temperature with windage, and is subject to small aerolite, the hypervelocity impact of space debris, and the corrosion of near-earth atmosphere 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 ceramics, top plate, lower plywood, phase-change material, shell and ceramic wafer, 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 ceramics, 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 connected mode of honeycomb ceramics and top plate, lower plywood is high temperature vacuum brazing. Fe base ODS alloy still has very high elevated temperature strength, high temperature creep property and antioxygenic 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 serviceability 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 ceramics 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 antioxygenic property and weldability, a kind of preparation method of large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material is provided.
Large scale 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%Y2O3And the Fe of aequum composition, opposite side by weight percentage composition by 15.0%-40.0%Cr, 0%-5.0%Al, 0.3%-0.6%Y2O3And the Fe of aequum composition.
The preparation method of large scale 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 yittrium oxide powder are put into another water jacketed copper crucible, in yittrium oxide ingot surface, place 10-15 gram of calcirm-fluoride, high-temperature alloy base sheet is installed on frame substrate, use absolute ethyl alcohol wipe surfaces, be evacuated to 1 × 10-3Pa-5×10-3Pa, is then heated to 650-1000 DEG C by high temperature alloy substrate, insulation;
Two, adopt baffle plate to block the high temperature alloy 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 high temperature alloy substrate, deposit thickness is the CaF of 1-10 μ m2；
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 yittrium oxide powder 10-60min, is 1 × 10 in vacuum-3Pa-5×10-3Under the condition of Pa, naturally cool to 50 DEG C, obtain large scale 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 scale 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 ceramics.
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 scale, easily welds anti-oxidant gradient aluminium content ferrum-chromium-aluminum ODS latten material, than the iron-base superalloy light sheet material thin thickness of existing same size, iron-base superalloy light sheet material size than existing same thickness is large, antioxygenic property than the iron-base superalloy light sheet 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, antioxygenic property is good, and (in 1100 DEG C of 100h air, oxidation weight gain is not higher than 0.8mg/cm2)；
(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 plate 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 scale 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 ceramics, and 6 represent thermal protection system metal honeycomb structure lower plywood.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: present embodiment large scale 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%Y2O3And the Fe of aequum composition, opposite side by weight percentage composition by 15.0%-40.0%Cr, 0%-5.0%Al, 0.3%-0.6%Y2O3And the Fe of aequum composition.
Detailed description of the invention two: described in detailed description of the invention one, the preparation method of large scale 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 yittrium oxide powder are put into another water jacketed copper crucible, in yittrium oxide ingot surface, place 10-15 gram of calcirm-fluoride, high-temperature alloy base sheet is installed on frame substrate, use absolute ethyl alcohol wipe surfaces, be evacuated to 1 × 10-3Pa-5×10-3Pa, is then heated to 650-1000 DEG C by high temperature alloy substrate, insulation;
Two, adopt baffle plate to block the high temperature alloy 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 high temperature alloy substrate, deposit thickness is the CaF of 1-10 μ m2；
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 yittrium oxide powder 10-60min, is 1 × 10 in vacuum-3Pa-5×10-3Under the condition of Pa, naturally cool to 50 DEG C, obtain large scale 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.
Detailed description of the invention three: what present embodiment was different from detailed description of the invention two is to be evacuated to 3 × 10 in step 1-3Pa. Other is identical with detailed description of the invention two.
Detailed description of the invention four: what present embodiment was different from detailed description of the invention two or three is, in step 1, high temperature alloy substrate is heated to 660 DEG C, insulation. Other is identical with detailed description of the invention two or three.
Detailed description of the invention five: what present embodiment was different from one of detailed description of the invention 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 detailed description of the invention two to four.
Detailed description of the invention six: what present embodiment was different from one of detailed description of the invention 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 detailed description of the invention two to five.
Detailed description of the invention seven: what present embodiment was different from one of detailed description of the invention two to six is to adopt 1.2A electron beam current evaporation oxidation yttrium pottery ingot or yittrium oxide powder 30min in step 3. Other is identical with one of detailed description of the invention two to six.
Detailed description of the invention eight: what present embodiment was different from one of detailed description of the invention two to seven is to adopt 1A electron beam current evaporation oxidation yttrium pottery ingot or yittrium oxide powder 40min in step 3. Other is identical with one of detailed description of the invention two to seven.
Detailed description of the invention nine: the large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material described in one of detailed description of the invention 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 ceramics.
Adopt following experimental verification effect of the present invention:
Experiment one:
The preparation method of large scale 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 calcirm-fluoride, high-temperature alloy base sheet is installed on frame substrate, use absolute ethyl alcohol wipe surfaces, be evacuated to 2 × 10-3Pa, is then heated to 660 DEG C by high temperature alloy substrate, insulation;
Two, adopt baffle plate to block the high temperature alloy 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 high temperature alloy substrate, deposit thickness is the CaF of 1-10 μ m2；
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 yittrium oxide powder 30min, is 3 × 10 in vacuum-3Under the condition of Pa, naturally cool to 50 DEG C, obtain large scale 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 high temperature alloy described in step 1 is 1000mm.
The large scale 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 ceramics, 6 represent thermal protection system metal honeycomb structure lower plywood, the large scale 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 ceramics, the large scale 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 ceramics, under high alumina one side direction.
Experiment two:
The preparation method of large scale 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 calcirm-fluoride, 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 absolute ethyl alcohol wipe surfaces, be evacuated to 4 × 10-3Pa, is then heated to 800 DEG C by high temperature alloy substrate, insulation;
Two, adopt baffle plate to block the high temperature alloy 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 high temperature alloy substrate, deposit thickness is the CaF of 1-10 μ m2；
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-3Under the condition of Pa, naturally cool to 50 DEG C, obtain large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material;
The diameter of the substrate of high temperature alloy described in step 1 is 1000mm.
The large scale 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 ceramics, 6 represent thermal protection system metal honeycomb structure lower plywood, the large scale 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 ceramics, the large scale 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 ceramics, under high alumina one side direction.
Experiment three:
The preparation method of large scale 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 calcirm-fluoride, 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 absolute ethyl alcohol wipe surfaces, be evacuated to 2 × 10-3Pa, is then heated to 900 DEG C by high temperature alloy substrate, insulation;
Two, adopt baffle plate to block the high temperature alloy 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 high temperature alloy substrate, deposit thickness is the CaF of 1-10 μ m2；
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-3Under the condition of Pa, naturally cool to 50 DEG C, obtain large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material;
The diameter of the substrate of high temperature alloy described in step 1 is 1000mm.
The large scale 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 ceramics, 6 represent thermal protection system metal honeycomb structure lower plywood, the large scale 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 ceramics, the large scale 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 ceramics, under high alumina one side direction.
Claims (1)
1. the preparation method of large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material, is characterized in that the preparation method of large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material carries out according to following steps:
The FeCrAl-Al sandwich ingot of 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 calcirm-fluoride, high-temperature alloy base sheet is installed on frame substrate, use absolute ethyl alcohol wipe surfaces, be evacuated to 2 × 10-3Pa, is then heated to 660 DEG C by high temperature alloy substrate, insulation;
Two, adopt baffle plate to block the high temperature alloy substrate through step 1 processing, two electron beam currents are increased to respectively to 2.8A and 1.3A, open baffle plate in the time that molten bath appears in ingot surface, on high temperature alloy substrate, deposit thickness is the CaF of 1-10 μ m2；
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 yittrium oxide powder 30min, is 3 × 10 in vacuum-3Under the condition of Pa, naturally cool to 50 DEG C, obtain large scale 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 high temperature alloy described in step 1 is 1000mm;
Described large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material thickness is 0.01-0.3mm, and diameter is 1000mm;
Described large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material high alumina one side aluminium content is 10.0wt.%-30.0wt.%, at 1100 DEG C in 100h air oxidation weight gain not higher than 0.8mg/cm2; The low aluminium one side aluminium content of large scale gradient aluminium content ferrum-chromium-aluminum ODS latten material is 0wt.%-5.0wt.%.
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