CN115404373B - Method for preparing in-situ synthesis aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material - Google Patents
Method for preparing in-situ synthesis aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material Download PDFInfo
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- CN115404373B CN115404373B CN202211233536.9A CN202211233536A CN115404373B CN 115404373 B CN115404373 B CN 115404373B CN 202211233536 A CN202211233536 A CN 202211233536A CN 115404373 B CN115404373 B CN 115404373B
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 117
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 87
- 239000010936 titanium Substances 0.000 title claims abstract description 75
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 75
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 35
- 239000002648 laminated material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 title claims description 10
- 238000003786 synthesis reaction Methods 0.000 title claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 47
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims description 65
- 229910002804 graphite Inorganic materials 0.000 claims description 39
- 239000010439 graphite Substances 0.000 claims description 39
- 239000011812 mixed powder Substances 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 19
- OQPDWFJSZHWILH-UHFFFAOYSA-N [Al].[Al].[Al].[Ti] Chemical compound [Al].[Al].[Al].[Ti] OQPDWFJSZHWILH-UHFFFAOYSA-N 0.000 claims description 15
- 229910021324 titanium aluminide Inorganic materials 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 11
- 239000000498 cooling water Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000005056 compaction Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 239000011268 mixed slurry Substances 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000012512 characterization method Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- TWHBEKGYWPPYQL-UHFFFAOYSA-N aluminium carbide Chemical compound [C-4].[C-4].[C-4].[Al+3].[Al+3].[Al+3].[Al+3] TWHBEKGYWPPYQL-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- 238000005086 pumping Methods 0.000 description 6
- 238000003475 lamination Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- ZOTQKIDWBQQTAL-UHFFFAOYSA-N alumane titanium Chemical compound [AlH3].[AlH3].[AlH3].[Ti] ZOTQKIDWBQQTAL-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 229910004349 Ti-Al Inorganic materials 0.000 description 1
- 229910004692 Ti—Al Inorganic materials 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- ZBZHVBPVQIHFJN-UHFFFAOYSA-N trimethylalumane Chemical compound C[Al](C)C.C[Al](C)C ZBZHVBPVQIHFJN-UHFFFAOYSA-N 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/004—Filling molds with powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
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- C22C—ALLOYS
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- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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Abstract
The invention relates to a method for preparing an in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material, which aims at the situation of the background technology and takes graphene, aluminum and titanium as raw materials to prepare the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material. The preparation method has advanced process, strict working procedures and high production efficiency, the prepared in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material is a cylindrical block, the hardness reaches 319HV, the tensile strength reaches 639.4MPa, the elongation reaches 10.6 percent, the aluminum carbide is uniformly dispersed in a matrix, and the titanium and aluminum laminated interface is well combined, so the preparation method is the advanced preparation method of the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material.
Description
Technical Field
The invention relates to a preparation method of an in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material, belonging to the technical field of preparation of a laminated structure material.
Background
The laminated material has a laminated structure, is formed by alternately laminating and connecting components with different components, has the performance characteristics of each component, and is a laminated structure material capable of simultaneously improving the strength and the plasticity of the material. The aluminum/titanium laminated material integrates the characteristics of light weight and high strength of titanium and the advantages of light weight and high plasticity of aluminum, and has wide application prospect. However, the hardness and strength of the aluminum layer is relatively low compared to the titanium layer, which is detrimental to the overall performance of the laminate. In addition, the physical parameters of titanium and aluminum are different, so that the heterogeneous interface of the laminated material is low in bonding strength and easy to crack in the service process. Therefore, the strength of the aluminum layer is improved, the combination between the titanium and the aluminum lamination is enhanced, the overall performance of the aluminum/titanium lamination material can be enhanced, and the application field of the aluminum/titanium lamination material is widened.
The aluminum carbide has a melting point of 2100 ℃ and a density of 2.97g/cm 3 The elastic modulus can reach 135GPa, and the aluminum layer can be used as a reinforcing phase to effectively improve the strength of the aluminum layer in the laminated material. However, conventional aluminum carbide is large in size, fails to exhibit a reinforcing effect effectively, and is difficult to be uniformly dispersed in a matrix. How to introduce the small-sized aluminum carbide to promote the aluminum carbide to be uniformly dispersed in the matrix is a difficult problem in preparation. The density of the titanium aluminide is 3.4g/cm 3 The oxidation resistance is the best in the common Ti-Al binary intermetallic compound, and the Young modulus is as high as 216GPa, so that the performance and the interface bonding strength of the laminated material can be improved. However, titanium aluminide formation tends to cause void defects within the laminate material. How to introduce titanium aluminide and avoid defects is a difficult preparation problem. Currently, the preparation of in-situ synthesized aluminum carbide and titanium trialuminum reinforced aluminum/titanium laminated materials from graphene, aluminum and titanium as raw materials is still in a research stage.
Disclosure of Invention
Object of the Invention
The invention aims to prepare an in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material by taking graphene, aluminum and titanium as raw materials aiming at the situation of the background art, so as to solve the problems of low strength of an aluminum layer, difficulty in uniform dispersion of aluminum carbide in a matrix and low bonding strength between laminated layers in the existing aluminum/titanium laminated material.
Technical scheme
The chemical substance materials used in the invention are as follows: graphene, aluminum, titanium, absolute ethyl alcohol and deionized water, wherein the combined preparation dosage is as follows: taking g and ml as measurement unit
Graphene: c solid powder 0.5g +/-0.001 g
Aluminum powder: 100 g. + -. 0.001g of Al solid powder
Titanium powder: ti solid powder 100g + -0.001 g
Absolute ethanol: c 2 H 5 OH liquid 1000mL +/-10 mL
Deionized water: h 2 O liquid 1000mL +/-10 mL
The preparation method comprises the following steps:
1) Ultrasonic dispersion
Weighing 0.5g +/-0.001 g of graphene, weighing 400mL of deionized water, adding the deionized water into a beaker with the capacity of 500mL, and rotationally stirring the mixture by using a glass rod; then, putting the beaker into an ultrasonic oscillator for ultrasonic dispersion, wherein the oscillation frequency is 900w, and the dispersion time is 1.5h, so as to prepare the graphene dispersion liquid;
2) Mixed powder
Weighing 99.5g of aluminum powder, weighing 500mL of absolute ethyl alcohol, adding into a beaker with the capacity of 1000mL, and uniformly stirring to obtain aluminum powder slurry; then, adding the graphene dispersion liquid into a beaker filled with aluminum powder slurry, and mechanically stirring at the stirring speed of 200r/min for 70min to prepare mixed slurry;
3) Drying by baking
Putting the beaker filled with the mixed slurry into a vacuum drying oven for drying at 70 ℃ for 24 hours to obtain graphene/aluminum mixed powder;
4) Powder stacking
Inserting a first pressure head of the discharge plasma sintering furnace into a graphite die, and placing a layer of graphite paper on the first pressure head; then, 5g of titanium powder is weighed and laid on graphite paper to form a first titanium powder layer; then, 3g of graphene/aluminum mixed powder is weighed and laid on a first titanium powder layer to form a first graphene/aluminum mixed powder layer; then, weighing 5g of titanium powder, and laying the titanium powder on the first graphene/aluminum mixed powder layer to form a second titanium powder layer; then, 3g of graphene/aluminum mixed powder is weighed and laid on a second titanium powder layer to form a second graphene/aluminum mixed powder layer; then, weighing 5g of titanium powder, and laying the titanium powder on a second graphene/aluminum mixed powder layer to form a third titanium powder layer; then, inserting a second pressure head of the discharge plasma sintering furnace into the graphite mold, and pressing a third titanium powder layer by using the second pressure head;
5) Powder compaction
After the graphite mold is fixed, the furnace door is closed, and the air in the furnace chamber is pumped out by a vacuum pump; then, starting a pressurizing device of the discharge plasma sintering furnace, and compacting three titanium powder layers and two graphene/aluminum mixed powder layers in the graphite die, wherein the pressure is 50MPa, and the compacting time is 5min;
6) Sintering and forming
Keeping the pressure intensity at 50MPa, starting a plasma discharge device, and performing discharge sintering on three titanium powder layers and two graphene/aluminum mixed powder layers in a graphite die at the sintering temperature of 550 ℃, the sintering time of 10min, and the sintering temperature rise rate of less than or equal to 100 ℃/min, so that the three titanium powder layers and the two graphene/aluminum mixed powder layers in the graphite die are sintered into a block body;
7) In-situ synthesis of aluminium carbide
Adjusting the pressure to 0MPa, and performing discharge sintering on the block in the graphite mold, wherein the sintering temperature is 620 ℃, the sintering time is 60min, and the sintering temperature rise rate is less than or equal to 100 ℃/min, so that the graphene in the block is converted into aluminum carbide;
8) Formation of titanium aluminide
Adjusting the pressure to 0.5MPa, continuing to perform discharge sintering on the block in the graphite die, wherein the sintering temperature is 700 ℃, the sintering time is 120min, and the sintering temperature rise rate is less than or equal to 100 ℃/min, so that atomic diffusion occurs at the interface of titanium and aluminum in the block to generate titanium aluminide, and the block is sintered into an in-situ synthesized aluminum carbide and titanium aluminide reinforced aluminum/titanium laminated material; then, the pressurizing device and the plasma discharge device of the discharge plasma sintering furnace are closed, and the furnace body of the discharge plasma sintering furnace is cooled by cooling water; opening the furnace door, and taking out the in-situ synthesized aluminum carbide and titanium trialuminum enhanced aluminum/titanium laminated material in the graphite mold;
9) Cleaning and rinsing
Cleaning the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material by using absolute ethyl alcohol, and drying after cleaning;
10 Detection, analysis, characterization
Detecting, analyzing and representing the appearance, color, microstructure and mechanical property of the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material;
carrying out microscopic structure analysis by using a field emission scanning electron microscope;
performing hardness analysis by using a Vickers hardness tester;
testing the tensile property by using an electronic universal testing machine;
and (4) conclusion: the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material is a cylindrical block, the hardness reaches 319HV, the tensile strength reaches 639.4MPa, the elongation reaches 10.6 percent, the aluminum carbide is uniformly dispersed in a matrix, and the titanium and aluminum laminated interface is well combined.
Advantageous effects
Compared with the background technology, the method has obvious advancement, aims at the conditions that the strength of an aluminum layer in the existing aluminum/titanium laminated material is low, aluminum carbide is difficult to be uniformly dispersed in a matrix, and the bonding strength between the laminated layers is low, takes graphene, aluminum and titanium as raw materials, and prepares the in-situ synthesized aluminum carbide and titanium aluminide reinforced aluminum/titanium laminated material by ultrasonic dispersion, powder mixing, drying, powder stacking, powder compacting, sintering and forming, in-situ synthesized aluminum carbide and titanium aluminide. The preparation method has advanced process, strict working procedures and high production efficiency, the prepared in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material is a cylindrical block, the hardness reaches 319HV, the tensile strength reaches 639.4MPa, the elongation reaches 10.6 percent, the aluminum carbide is uniformly dispersed in a matrix, and the titanium and aluminum laminated interface is well combined, so the preparation method is the advanced preparation method of the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material.
Drawings
FIG. 1 is a diagram showing the state of powder compaction, sintering and in-situ synthesis of aluminum carbide.
Fig. 2 is a view showing a state where powders are stacked.
FIG. 3 is a microstructure view of an in situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminate.
FIG. 4 is a tensile test plot of in situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminate.
As shown in the figures, the list of reference numbers is as follows:
1-a PLC control cabinet, 2-a control cabinet switch, 3-an alarm, 4-a pressure control knob, 5-a temperature control knob, 6-a time control knob, 7-a vacuum control knob, 8-a signal line, 9-a cooling water inlet, 10-a cooling water outlet, 11-a vacuum pump, 12-a vacuum-pumping valve, 13-a furnace body of a discharge plasma sintering furnace, 14-an upper hydraulic station, 15-a lower hydraulic station, 16-a conical head, 17-a pressure bar, 18-a current transmission device cathode, 19-a current transmission device anode, 20-a graphite mold of a discharge plasma sintering furnace, 21-a pressure head, 22-a titanium powder layer, 23-graphene/aluminum mixed powder layer, 24-graphite paper, 25-a temperature measurement hole, 26-a thermocouple, 27-a vacuum breaking valve, 28-a vacuum gauge, 29-an anode copper wire row, 30-a cathode copper wire row, 31-a high-frequency power supply anode, 32-a high-frequency power supply cathode, 33-a power supply switch, 34-a voltage control cabinet switch, and 35-a high-frequency power supply cabinet.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is a diagram showing the state of powder compaction, sintering and forming and in-situ synthesis of aluminum carbide; the whole set of equipment comprises a discharge plasma sintering furnace, a PLC control cabinet 1, a vacuum pump 11, a vacuum pumping valve 12, a vacuum breaking valve 27 and a vacuum meter 28;
a furnace body 13 of the discharge plasma sintering furnace is respectively provided with a cooling water inlet 9 and a cooling water outlet 10;
a temperature measuring hole 25 is arranged on the graphite mould 20 of the discharge plasma sintering furnace; a thermocouple 26 is inserted in the temperature measuring hole 25;
the pressurizing device of the discharge plasma sintering furnace comprises an upper hydraulic station 14, a lower hydraulic station 15, two conical heads 16, two pressure rods 17 and two pressure heads 21;
the plasma discharge device of the discharge plasma sintering furnace comprises a current transmission device cathode 18, a current transmission device anode 19, an anode copper wire row 29, a cathode copper wire row 30, a high-frequency power supply anode 31, a high-frequency power supply cathode 32 and a high-frequency power supply cabinet 35; a power supply cabinet switch 33 and a voltage control knob 34 are respectively arranged on the high-frequency power supply cabinet 35;
the PLC control cabinet 1 is connected with a pressurizing device of the discharge plasma sintering furnace through a signal wire 8; the PLC control cabinet 1 is respectively provided with a control cabinet switch 2, an alarm 3, a pressure control knob 4, a temperature control knob 5, a time control knob 6 and a vacuum control knob 7;
the vacuum pump 11 is communicated with the furnace chamber of the discharge plasma sintering furnace through a vacuum pumping valve 12;
the vacuum breaking valve 27 and the vacuum meter 28 are both communicated with a furnace chamber of the discharge plasma sintering furnace;
in the process of powder compaction, the furnace door is closed, the vacuum-pumping valve 12 is opened, the vacuum pump 11 is started through the vacuum control knob 7, the vacuum pump 11 is used for pumping the air in the furnace cavity, and the vacuum degree is monitored by the vacuum gauge 28; then, the PLC control cabinet 1 is started through a control cabinet switch 2, and an upper hydraulic station 14 and a lower hydraulic station 15 are started through a pressure control knob 4; the upper hydraulic station 14 and the lower hydraulic station 15 respectively push the two pressure rods 17 to move oppositely, the two pressure rods 17 respectively drive the two conical heads 16 to move oppositely, the two conical heads 16 respectively drive the two pressure heads 21 to move oppositely, and the two pressure heads 21 jointly compact three titanium powder layers 22 and two graphene/aluminum mixed powder layers 23 in the graphite mold 20;
in the sintering and forming process, a high-frequency power supply cabinet 35 is started through a power supply cabinet switch 33, output voltage is set through a voltage control knob 34, sintering temperature and sintering time are set through a temperature control knob 5 and a time control knob 6, current output by the high-frequency power supply cabinet 35 sequentially flows through a high-frequency power supply anode 31, an anode copper wire row 29, a current transmission device anode 19, a graphite mold 20 of a discharge plasma sintering furnace, a current transmission device cathode 18, a cathode copper wire row 30 and a high-frequency power supply cathode 32, three titanium powder layers 22 and two graphene/aluminum mixed powder layers 23 in the graphite mold 20 are sintered when flowing through the graphite mold 20 of the discharge plasma sintering furnace, and the sintering temperature is monitored by a thermocouple 26, so that the three titanium powder layers 22 and the two graphene/aluminum mixed powder layers 23 in the graphite mold 20 are sintered into a block;
in the process of synthesizing aluminum carbide in situ, the pressure intensity is adjusted by a pressure control knob 4, the sintering temperature and the sintering time are adjusted by a temperature control knob 5 and a time control knob 6, the current output by a high-frequency power supply cabinet 35 sequentially flows through a high-frequency power supply anode 31, an anode copper wire row 29, a current transmission device anode 19, a graphite mold 20 of a discharge plasma sintering furnace, a current transmission device cathode 18, a cathode copper wire row 30 and a high-frequency power supply cathode 32, the block in the graphite mold 20 is sintered when flowing through the graphite mold 20 of the discharge plasma sintering furnace, and the sintering temperature is monitored by a thermocouple 26, so that the graphene in the block is converted into aluminum carbide;
in the process of generating titanium aluminide, the pressure intensity is increased through the pressure control knob 4, the sintering temperature is increased and the sintering time is prolonged through the temperature control knob 5 and the time control knob 6, and the block in the graphite mold 20 is continuously sintered, so that atomic diffusion occurs at the interface of titanium and aluminum in the block to generate titanium aluminide, and the block is sintered into in-situ synthesized aluminum carbide and titanium aluminide reinforced aluminum/titanium laminated material; then, the upper hydraulic station 14 and the lower hydraulic station 15 are closed through the pressure control knob 4, the high-frequency power supply cabinet 35 is closed through the power supply cabinet switch 33, cooling water is introduced into the cooling water inlet 9, and the cooling water cools the furnace body 13 of the discharge plasma sintering furnace and is discharged through the cooling water outlet 10; then, the vacuum pump 11 is turned off, the vacuum-pumping valve 12 is closed, the vacuum breaking valve 27 is opened, air is introduced into the chamber of the spark plasma sintering furnace, the door of the furnace is opened, and the in-situ synthesized aluminum carbide and titanium trialuminide reinforced aluminum/titanium laminated material in the graphite mold 20 is taken out.
FIG. 2 is a view showing a state where powders are stacked;
during the powder stacking process, a first pressure head 21 of the discharge plasma sintering furnace is inserted into a graphite die 20, and a layer of graphite paper 24 is placed on the first pressure head 21; then, laying the weighed titanium powder on graphite paper 24 to form a first titanium powder layer 22, laying the weighed graphene/aluminum mixed powder on the first titanium powder layer 22 to form a first graphene/aluminum mixed powder layer 23, laying the weighed titanium powder on the first graphene/aluminum mixed powder layer 23 to form a second titanium powder layer 22, laying the weighed graphene/aluminum mixed powder on the second titanium powder layer 22 to form a second graphene/aluminum mixed powder layer 23, and laying the weighed titanium powder on the second graphene/aluminum mixed powder layer 23 to form a third titanium powder layer 22; then, the second indenter 21 of the discharge plasma sintering furnace is inserted into the graphite mold 20, and the third layer of titanium powder 22 is pressed with the second indenter 21.
FIG. 3 is a microstructure diagram of an in situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminate; as shown in the figure, the lamination interfaces of the material are well combined, no air holes or crack defects exist, uniform titanium aluminide is generated at the interface of the titanium layer and the aluminum layer, and large aluminum carbide particles are not seen in the microstructure of the material, so that the size of the aluminum carbide is small, and the aluminum carbide is uniformly dispersed in the matrix.
FIG. 4 is a drawing of a tensile test of in situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminate; as shown in the figure, the tensile strength of the material reaches 639.4MPa, the elongation reaches 10.6%, and the tensile property is good.
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and that the scope of the invention is defined by the appended claims. Various changes or modifications to these embodiments can be made by those skilled in the art without departing from the principle and spirit of this invention, and these changes and modifications all fall into the scope of this invention.
Claims (1)
1. A method for preparing an aluminum/titanium laminated material enhanced by in-situ synthesis of aluminum carbide and titanium trialuminate is characterized by comprising the following steps:
the chemical materials used were: graphene, aluminum, titanium, absolute ethyl alcohol and deionized water, wherein the combined preparation dosage is as follows: taking g and ml as measurement unit
Graphene: c solid powder 0.5 g. + -. 0.001g
Aluminum powder: al solid powder 100 g. + -. 0.001g
Titanium powder: ti solid powder 100 g. + -. 0.001g
Anhydrous ethanol: c 2 H 5 OH liquid 1000mL +/-10 mL
Deionized water: h 2 O liquid 1000mL +/-10 mL
The preparation method comprises the following steps:
1) Ultrasonic dispersion
Weighing 0.5g +/-0.001 g of graphene, weighing 400mL of deionized water, adding the deionized water into a beaker with the capacity of 500mL, and rotationally stirring the mixture by using a glass rod; then, putting the beaker into an ultrasonic oscillator for ultrasonic dispersion, wherein the oscillation frequency is 900w, and the dispersion time is 1.5h, so as to prepare the graphene dispersion liquid;
2) Mixed powder
Weighing 99.5g of aluminum powder, weighing 500mL of absolute ethyl alcohol, adding the absolute ethyl alcohol into a beaker with the capacity of 1000mL, and uniformly stirring to obtain aluminum powder slurry; then, adding the graphene dispersion liquid into a beaker filled with aluminum powder slurry, and mechanically stirring at the stirring speed of 200r/min for 70min to prepare mixed slurry;
3) Drying the mixture
Putting the beaker filled with the mixed slurry into a vacuum drying oven for drying at 70 ℃ for 24 hours to obtain graphene/aluminum mixed powder;
4) Powder stacking
Inserting a first pressure head of the discharge plasma sintering furnace into a graphite die, and placing a layer of graphite paper on the first pressure head; then, 5g of titanium powder is weighed and laid on graphite paper to form a first titanium powder layer; then, 3g of graphene/aluminum mixed powder is weighed and laid on a first titanium powder layer to form a first graphene/aluminum mixed powder layer; then, 5g of titanium powder is weighed and laid on the first graphene/aluminum mixed powder layer to form a second titanium powder layer; then, 3g of graphene/aluminum mixed powder is weighed and laid on a second titanium powder layer to form a second graphene/aluminum mixed powder layer; then, weighing 5g of titanium powder, and laying the titanium powder on a second graphene/aluminum mixed powder layer to form a third titanium powder layer; then, inserting a second pressure head of the discharge plasma sintering furnace into the graphite mold, and pressing a third titanium powder layer by using the second pressure head;
5) Powder compaction
After the graphite mold is fixed, the furnace door is closed, and the air in the furnace chamber is pumped out by a vacuum pump; then, starting a pressurizing device of the discharge plasma sintering furnace, and compacting three titanium powder layers and two graphene/aluminum mixed powder layers in the graphite mold, wherein the pressure is 50MPa, and the compacting time is 5min;
6) Sintering and forming
Keeping the pressure intensity at 50MPa, starting a plasma discharge device, and performing discharge sintering on three titanium powder layers and two graphene/aluminum mixed powder layers in a graphite die at the sintering temperature of 550 ℃, the sintering time of 10min, and the sintering temperature rise rate of less than or equal to 100 ℃/min, so that the three titanium powder layers and the two graphene/aluminum mixed powder layers in the graphite die are sintered into a block;
7) In-situ synthesis of aluminium carbide
Adjusting the pressure to be 0MPa, and performing discharge sintering on the block in the graphite mold, wherein the sintering temperature is 620 ℃, the sintering time is 60min, and the sintering temperature rise rate is less than or equal to 100 ℃/min, so that the graphene in the block is converted into aluminum carbide;
8) Formation of titanium aluminide
Adjusting the pressure to 0.5MPa, continuing to perform discharge sintering on the block in the graphite die, wherein the sintering temperature is 700 ℃, the sintering time is 120min, and the sintering temperature rise rate is less than or equal to 100 ℃/min, so that atomic diffusion occurs at the interface of titanium and aluminum in the block to generate titanium aluminide, and the block is sintered into an in-situ synthesized aluminum carbide and titanium aluminide reinforced aluminum/titanium laminated material; then, the pressurizing device and the plasma discharge device of the discharge plasma sintering furnace are closed, and the furnace body of the discharge plasma sintering furnace is cooled by cooling water; opening the furnace door, and taking out the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material in the graphite mold;
9) Cleaning and rinsing
Cleaning the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material by using absolute ethyl alcohol, and drying after cleaning;
10 Detection, analysis, characterization
Detecting, analyzing and representing the appearance, color, microstructure and mechanical property of the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material;
carrying out microscopic structure analysis by using a field emission scanning electron microscope;
performing hardness analysis by using a Vickers hardness tester;
testing the tensile property by using an electronic universal testing machine;
and (4) conclusion: the in-situ synthesized aluminum carbide and titanium trialuminate reinforced aluminum/titanium laminated material is a cylindrical block, the hardness reaches 319HV, the tensile strength reaches 639.4MPa, the elongation reaches 10.6 percent, the aluminum carbide is uniformly dispersed in a matrix, and the titanium and aluminum laminated interface is well combined.
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