CN1877315A - Measurement method for seepage characteristic of metal-based composite material prepared by vacuum negative pressure impregnation - Google Patents
Measurement method for seepage characteristic of metal-based composite material prepared by vacuum negative pressure impregnation Download PDFInfo
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Abstract
The invention discloses a method for measuring filtration performance of metal compound material, which comprises inserting two tungsten wires or 13 probes into perform, drying in low temperature and adglutinating in high temperature for back up; when measuring the imbibition height of the high temperature metal, placing the perform with tungsten wires in the quartz crucible, wherein the tungsten wires are connected with the external interface circuit via lead wires, the molten metal liquid filtrates upwards under the action of negative pressure and dipping in the perform; the external interface circuit collect card recording the voltage variation process, getting the relationship curve of the filtration liquid surface offset versus time.
Description
Technical field
The present invention relates to a kind of metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic.
Background technology
Widespread use along with metal-base composites, be the research background based on various different reinforcing materials, matrix material, the preparation and the manufacturing process of multiple metal-base composites have been developed, as spray co deposition method, powder metallurgic method, diffusion connection method, stirring casting method, in-situ reaction etc.The negative pressure of vacuum method of impregnation is one of effective method of preparation metal-base composites, can satisfy the near-net-shape of member, its ultimate principle is a heating and melting under vacuum condition,, treat to obtain metal-base composites after liquid metal under low pressure solidifies with in the reverse infiltrated fiber precast body of molten metal by gas pressure difference.Wherein, the flow event of liquid metal in porous medium determined the negative pressure of vacuum method of impregnation to prepare the apparent size and the inner structure of metal-base composites, is this technology key of success.Because preparation process is at high temperature carried out, the seepage flow phenomenon and the basic law of its liquid metal, all be difficult to observation as free face, seepage flow forward position shape, percolation flow velocity and Changing Pattern thereof etc., be difficult to study the reciprocation of technological parameter to the inhomogeneity influence of infiltrating, be difficult for correctly, reasonably formulating technological parameter, thereby be difficult to the effective control of realization preparation process.Up to the present, choosing of technological parameter mainly is the practical experience that relies on the operator, and it is very big to implement difficulty.Therefore, be necessary to explore suitable high-temperature liquid metal negative pressure measurement method for seepage characteristic, so as under the research different technology conditions molten metal percolation law, thereby reach the purpose of effective control metal-base composites forming quality.
Document " application number is 93111553.1 Chinese patent " has been introduced the infiltration analogue method for making of a kind of metal-base composites and porous metals, this method is utilized the fluid principle of similitude that flows, select under the room temperature the identical liquid of liquid metal viscosity in its viscosity and prototype for use, in the transparent organic glass model of filler particles is housed, simulation liquid metal flow event.The instantaneous pressure measurement of the Seepage Flow Simulation Test Unit that analog machine is made by transparent organic glass, control pressurer system and flow event system forms.The instantaneous pressure measurement of flow event system is by sensor, form from stream amplifier, magnetic tape recorder, A/D conversion equipment, computing machine and plotting apparatus.Magnetic tape recorder can write down sensor high precision transient pressure to be changed.
This method is utilized the fluid principle of similitude that flows, at room temperature simulate the liquid metal flow event, still have the following disadvantages: have the difference of state parameters such as viscosity coefficient, wellability between selected room temperature liquid and the metal liquid, can't accurately measure molten metal infiltration process displacement---time curve; Can't qualitative description Free Surface of Seepage shape; Practical problems is simplified, be difficult to simulate that molten metal solidifies under the condition of high temperature in infiltration process, molten phenomenon is to the influence of infiltration speed again.
Summary of the invention
The deficiency that can not simulate in order to overcome prior art that molten metal solidifies under the condition of high temperature in infiltration process, there is obvious errors in molten phenomenon to the influence of infiltration speed and measured value and theoretical value again, the invention provides a kind of metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic, the infiltration liquid level be can measure and situation, the seepage flow basic law of quantitative test molten metal in porous preform advanced.
The technical solution adopted for the present invention to solve the technical problems is: a kind of metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic, it is characterized in that, and comprise the steps:
1) in the precast body biscuit, insert two tungsten filaments or 13 probes, standby behind low temperature drying and high temperature sintering;
2) when measuring high-temperature liquid metal infiltration height, the precast body that inserts tungsten filament is placed in the silica crucible, tungsten filament is connected with external interface circuit by wire column;
3) when measuring high-temperature liquid metal infiltration liquid level propelling situation, the precast body that inserts probe is placed in the silica crucible, probe is connected with external interface circuit by wire column;
4) start-up temperature control system, A electric resistance heater 13 heating 1.5 hours make the silica crucible temperature be controlled at 600 ± 5 ℃, and B electric resistance heater 16 heating 2 hours make the stainless steel crucible temperature be controlled at 800 ± 5 ℃, and the LY12 aluminium alloy is all melted; Furnace chamber is vacuumized, when vacuum tightness reaches 0.095MPa in the furnace chamber, stop to vacuumize; Promoting stainless steel crucible immerses in the molten aluminium alloy liquid silica crucible mouth of pipe; Give to feed inert gas in the furnace chamber, and the 100～500KPa that keep-ups pressure;
5) molten metal bath seepage flow upwards under suction function, be immersed in the precast body, along with molten metal constantly infiltrates, the change procedure of external interface circuit capture card synchronous recording voltage reaches steady state (SS) until system, draws voltage and time curve, utilize the similarity of the seepage field and the current field characteristics of motion, can get seepage liquid level displacement---time curve, the corresponding seepage distance of change in voltage, the corresponding infiltration speed of rate of voltage rise; In like manner, when the seepage liquid level order arrives tat probe difference contact, utilize the electric conductivity of metal, by the trigger circuit in the proving installation, capture card in time writes down the time that seepage liquid level arrives differing heights, adopts and gets the shape that a match can obtain Free Surface of Seepage.
The position of described tungsten filament in precast body is along precast body center pedal line, is symmetrically distributed at 1/2 place of section radius, and the tungsten filament upper/lower terminal all stretches out precast body.
The position of described probe in precast body be, along the vertical cross-section diameter, respectively uniform vertical is placed 7 probes, and precast body is stretched out in the upper end of probe, and the lower end is positioned at 1/2 place of precast body height.
The invention has the beneficial effects as follows, because continuous resistance measurement infiltration displacement of employing and time relation adopt distributed sonde method to measure the infiltration liquid level and advance situation, energy synthetic study high-temperature liquid metal negative pressure flow event and percolation law; Measure and at high temperature carry out, identical with the actual fabrication condition, can be more comprehensively, set up the infiltration height with infiltration time, infiltration pressure, precast body preheat temperature, fiber radius, the isoparametric relation of precast body volume fraction and solidify the influence that percolation flow velocity is produced exactly, provide foundation for choosing optimal processing parameter, help the control of flow event, reduce experimental cost and rejection rate that liquid THROUGH METHOD prepares composite technology, realize that the liquid THROUGH METHOD of negative pressure prepares the low cost of compound substance, the efficient manufacturing.
The present invention is further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the synoptic diagram of metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic isolated plant embodiment 1 of the present invention
Fig. 2 is the synoptic diagram of metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic isolated plant embodiment 2 of the present invention
Fig. 3 is metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic isolated plant embodiment 2 middle probes of the present invention distribution schematic diagrams in precast body
Among the figure, 1. guide rod, 2. wire column, 3. upper cover, 4. air intake valve, 5. bell, 6. gasket seal, 7. tungsten filament, 8. body of heater, 9. stainless steel crucible, 10. evacuating valve, 11. silica crucibles, 12. precast bodies, 13.A electric resistance heater, 14. supports, 15. molten metals, 16.B electric resistance heater, 17. push rods, 18. probes.
Embodiment
Embodiment 1, and with reference to Fig. 1, the used metallic matrix of the present invention is the LY12 aluminium alloy, the Al that precast body adopts Luoyang fire resistive material research institute to produce
2O
3Whisker, precast body are of a size of 58 * 52mm; Porosity is 32%.
Adopt wet method to prepare Al
2O
3During the whisker prefabricated component, be about to Al
2O
3Whisker, pore creating material, whisker spreading agent, bonding agent and distilled water mix by a certain percentage, after stirring, filter out moisture, compression molding, obtain the whisker preform biscuit after, two tungsten filaments are inserted in the precast body biscuits, behind low temperature drying and high temperature sintering, obtain presetting the Al of tungsten filament again
2O
3The whisker prefabricated component.In flow event, liquid level and die cavity wall are perpendicular, and the retainer shaft symmetry boosts along vertical, thus with tungsten filament along precast body center pedal line, be symmetrically distributed at 1/2 place of section radius, precast body 8mm is stretched out in the tungsten filament upper end, and precast body 5mm is stretched out in the lower end.
Guide rod 1 and upper cover 3 adopt self sealss to be threaded; Wire column 2 is inserted respectively in guide rod 1 and the upper cover 3, the wire column of guide rod 1 is connected with fine copper wire with wire column in the upper cover 3, two tungsten filaments 7 in the precast body 12 are connected with the wire column of guide rod 1 respectively, and the wire column in the upper cover 3 is connected with external interface circuit; The guide rod 1 and precast body 12 integral body of turning on the electricity are placed in the silica crucible 11; Silica crucible 11 and bell 5 adopt clearance fit; Use dormant bolt fastening after placing packing washer in the middle of upper cover 3 and the bell 5; Push rod 17 and body of heater 8 adopt self sealss to be threaded; Stainless steel crucible 9 is coaxial to be placed on the pallet of push rod 17, and pallet contacts with body of heater 8 bottoms; At stainless steel crucible 9 placed around B electric resistance heaters 16; Quantitative aluminium alloy LY12 is added in the stainless steel crucible 9, put support 14; Fixed placement A electric resistance heater 13 on support 14, heating precast body 12; Put gasket seal 6 in the middle of bell 5 and the body of heater 8, use bolted; The output line of tungsten filament 7 is connected in external interface circuit, and computing machine receives voltage change signal by external circuit.
Be linked and packed in a manner described finish after, close air intake valve 4, open evacuating valve 10, with vacuum pump furnace chamber is vacuumized, when vacuum tightness reaches 0.095MPa in the furnace chamber, stop to vacuumize, continue next step operation; Otherwise, check the sealing situation of each interface, be threaded in the mouth of pipe for self sealss and twine the rope made of hemp and strengthen its sealing, after finishing by top order of connection assembling, the operation below continuing.Close evacuating valve 10, the start-up temperature control system, A electric resistance heater 13 heating 1.5 hours make its temperature about 600 ℃, and B electric resistance heater 16 heating 2 hours make its temperature about 800 ℃, make the LY12 aluminium alloy all melt; Open evacuating valve 10, furnace chamber is vacuumized, when vacuum tightness reaches 0.095MPa in the furnace chamber, stop to vacuumize with vacuum pump; Motion push rod 17 promotes stainless steel crucible 9, and silica crucible 11 mouths of pipe are contacted with molten metal bath 15, closes evacuating valve 10, opens air intake valve 4, feeds nitrogen, regulates control pressurer system and makes the interior gaseous tension of furnace chamber remain on 250KPa; LY12 aluminum alloy melt seepage flow upwards under suction function, be immersed in the precast body, along with molten metal constantly infiltrates, the tungsten filament effective resistance reduces, and the measuring resistance both end voltage increases, the change procedure of capture card synchronous recording voltage, reach steady state (SS) until system, draw voltage and time curve, utilize the similarity of the seepage field and the current field characteristics of motion, get final product seepage liquid level displacement and time relation.The corresponding infiltration of change in voltage distance, the corresponding infiltration speed of rate of voltage rise.
Embodiment 3, the metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic: 1) tungsten filament 7 or distribution probe 18 are embedded in the precast body 12, precast body is stretched out at the tungsten filament two ends, and distribution probe one end stretches out precast body, connecting circuit and device seal furnace chamber;
2) start-up temperature control system, A electric resistance heater 13 heating 1.5 hours make silica crucible 11 temperature be controlled at 600 ± 5 ℃, and B electric resistance heater 16 heating 2 hours make stainless steel crucible 10 temperature be controlled at 800 ± 5 ℃, and the LY12 aluminium alloy is all melted;
3) start vacuum extractor, furnace chamber is vacuumized, when vacuum tightness reaches 0.095MPa in the furnace chamber, stop to vacuumize with vacuum pump;
4) promoting stainless steel crucible 10 immerses in the fusion LY12 aluminum alloy melt 15 silica crucible 12 mouths of pipe;
5) close evacuating valve 10, start the inert gas pressure control system, give to feed inert gas in the furnace chamber, and adjust pressure between 100～500KPa;
6) molten metal bath seepage flow upwards under suction function, be immersed in the precast body, along with molten metal constantly infiltrates: when adopting continuous electric-resistivity method, the tungsten filament effective resistance reduces, the measuring resistance both end voltage increases, the change procedure of capture card synchronous recording voltage, reach steady state (SS) until system, draw voltage and time curve, utilize the similarity of the seepage field and the current field characteristics of motion, can get seepage liquid level displacement---time relationship, the corresponding seepage distance of change in voltage, the corresponding infiltration speed of rate of voltage rise; When adopting the distribution sonde method, when the seepage liquid level order arrives tat probe difference contact, utilize the electric conductivity of metal, by the trigger circuit in the proving installation, capture card in time writes down the time that seepage liquid level arrives differing heights, adopts and gets the shape that a match can obtain Free Surface of Seepage.
Claims (3)
1, a kind of metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic is characterized in that, comprises the steps:
1) in the precast body biscuit, insert two tungsten filaments or 13 probes, standby behind low temperature drying and high temperature sintering;
2) when measuring high-temperature liquid metal infiltration height, the precast body that inserts tungsten filament is placed in the silica crucible, tungsten filament is connected with external interface circuit by wire column;
When measuring high-temperature liquid metal infiltration liquid level propelling situation, the precast body that inserts probe is placed in the silica crucible, probe is connected with external interface circuit by wire column;
3) start-up temperature control system, A electric resistance heater 13 heating 1.5 hours make the silica crucible temperature be controlled at 600 ± 5 ℃, and B electric resistance heater 16 heating 2 hours make the stainless steel crucible temperature be controlled at 800 ± 5 ℃, and the LY12 aluminium alloy is all melted; Furnace chamber is vacuumized, when vacuum tightness reaches 0.095MPa in the furnace chamber, stop to vacuumize; Promoting stainless steel crucible immerses in the molten aluminium alloy liquid silica crucible mouth of pipe; Give to feed inert gas in the furnace chamber, and the 100～500KPa that keep-ups pressure;
4) molten metal bath seepage flow upwards under suction function, be immersed in the precast body, along with molten metal constantly infiltrates, the change procedure of external interface circuit capture card synchronous recording voltage reaches steady state (SS) until system, draw voltage and time curve, match on theoretical plate utilizes the similarity of the seepage field and the current field characteristics of motion, can get seepage liquid level height---time curve, the corresponding seepage distance of change in voltage, the corresponding infiltration speed of rate of voltage rise; In like manner, when the seepage liquid level order arrives tat probe difference contact, utilize the electric conductivity of metal, by the trigger circuit in the proving installation, capture card in time writes down the time that seepage liquid level arrives differing heights, adopts and gets the shape that a match can obtain Free Surface of Seepage.
2, metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic according to claim 1, it is characterized in that: the position of described tungsten filament in precast body is along precast body center pedal line, is symmetrically distributed at 1/2 place of section radius, and the tungsten filament upper/lower terminal all stretches out precast body.
3, metal-based composite material prepared by vacuum negative pressure impregnation measurement method for seepage characteristic according to claim 1, it is characterized in that: the position of described probe in precast body is, along the vertical cross-section diameter, respectively uniform vertical is placed 7 probes, precast body is stretched out in the upper end of probe, and the lower end is positioned at 1/2 place of precast body height.
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