CN102363844B - Method for preparing pore gradient metal or alloy material by microwave sintering - Google Patents
Method for preparing pore gradient metal or alloy material by microwave sintering Download PDFInfo
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- CN102363844B CN102363844B CN2011103407957A CN201110340795A CN102363844B CN 102363844 B CN102363844 B CN 102363844B CN 2011103407957 A CN2011103407957 A CN 2011103407957A CN 201110340795 A CN201110340795 A CN 201110340795A CN 102363844 B CN102363844 B CN 102363844B
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Abstract
The invention relates to a method for preparing pore gradient metal or an alloy material by microwave sintering. The method comprises the following steps of: manufacturing a blank; putting the compacted blank into a heat-insulating cavity made of a heat-insulating material, wherein in the wall thickness of the heat-insulating cavity, one end is thin, and the other end is thick; and putting the compacted blank into a microwave high-temperature furnace, heating at a speed of 5 to 10 DEG C/minute to the temperature which is 0.7 time of sintering temperature Ts, then heating at a speed of 20 to 50 DEG C/minute to the sintering temperature, turning off a microwave source, and cooling with the furnace. In the method, alloy with a gradient structure is prepared by using a microwave sintering technology, and the gradient pore alloy material can be sintered in the ordinary microwave high-temperature furnace; and after the gradient pore alloy is obtained, the alloy material with gradient ingredients can be prepared by an infiltration process, and the integral process is easy to design, simple, controllable and low in cost. Compared with the conventional process, the method has the advantages that: the blank with the gradient structure is not needed to be manufactured before sintering; a gradient temperature field is formed by using a microwave selective heating technology; sintering effects of products in different areas are controlled; and a controllable gradient tissue structure is obtained. The method can be used for industrial production.
Description
Technical field:
The present invention relates to a kind of method for preparing porosity gradient metal or alloy material.Refer to especially a kind of method that adopts Microwave Sintering Techniques to prepare gradient-porosity metal or alloy material.Belong to microwave application and porosity gradient alloy preparing technical field.
Background technology
The technology of preparing of existing Functionally Graded Materials mainly contains plasma spraying, electrophoretic deposition, vapour deposition, certainly spreads the methods such as synthetic, laser sintered.These methods exist that complex process, equipment requirements are high, the high in cost of production shortcoming.
The principle of Microwave Sintering Techniques is micro-wave energy is converted into to heat energy and causes powder consolidation and alloying at material internal, is that a kind of volume adds thermal behavior, has that rate of heating is fast, the sintering period is short, energy expenditure is low and advantages of environment protection.It is generally acknowledged that the material structure that the material of microwave sintering obtains is more even than the normal sintering method.
The experiment of the Roy of Pennsylvania State Univ-Univ Park USA in 1999 etc. report microwave sintering iron-based powder metallurgy parts, prove that metal-powder can be by microwave sintering effectively.
Current research is thought, due to the volume effect of microwave heating, can make tiny even, the performance boost of material structure.On the other hand, it is selectivity heating that microwave sintering has another feature, that is: absorb when the different material of microwave ability heat in given microwave field and will obtain different heats, thisly because the different microwave heating behavior of material is called as selectivity, heats.
For metal-powder, can be drawn by classical Maxwell equation: the ability that metal-powder absorbs microwave raises along with temperature and strengthens.That is to say, metal-powder can be heated by microwave selective under given conditions.
But, utilize the microwave heating direct sintering to prepare the porosity gradient alloy material, so far there are no reports.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and provide a kind of processing method simple, easy to operate, can be in common industrial microwave High Temperature Furnaces Heating Apparatus the direct sintering microwave sintering for preparing the gradient-porosity alloy material prepare the method for porosity gradient metal or alloy material.By microwave sintering insulation construction and the microwave sintering process of particular design, in sintering process, form controlled thermograde, the difference of contraction, hole while utilizing thermograde to cause the alloy material sintering, form the gradient-structure alloy.
A kind of microwave sintering of the present invention prepares the method for porosity gradient metal or alloy material, comprises the steps:
The first step: base
Porosity gradient alloy compositions proportioning according to design, take each component, and powder metallurgy blank-making technology batch mixing, compression moulding, obtain pressed compact routinely;
Second step: pressed compact parcel
The pressed compact that the first step is obtained is placed in the incubation cavity of being made by lagging material, and wall thickness one end of described incubation cavity is thin, and an end is thick;
The 3rd step: sintering
The pressed compact that second step is wrapped is placed in the industrial microwave High Temperature Furnaces Heating Apparatus, regulates microwave output power, and the control pressed compact is warming up to 0.7 times of sintering temperature Ts with the speed of 5-10 ℃/min; Then, be warming up to sintering temperature with 20-50 ℃/min, close microwave source, furnace cooling.
Prepared in the method for porosity gradient metal or alloy material by a kind of microwave sintering of the present invention, the end that described incubation cavity is thin is provided with the heat radiation through hole.
Prepared in the method for porosity gradient metal or alloy material by a kind of microwave sintering of the present invention, the end that described incubation cavity is thick is placed with the boosting material, and the fusing point of described boosting material is higher 200 ℃ than sintering temperature.
Prepared in the method for porosity gradient metal or alloy material by a kind of microwave sintering of the present invention, described boosting material is SiC.
Prepared in the method for porosity gradient metal or alloy material by a kind of microwave sintering of the present invention, described lagging material is aluminum oxide lagging material or alumina-mullite lagging material.
Prepared in the method for porosity gradient metal or alloy material by a kind of microwave sintering of the present invention, described alloy is selected from a kind of in W, Fe, Cu, Ti, Al, Mo alloy.
Mechanism of the present invention sketch under: research thinks, due to the volume effect of microwave heating, can make that material structure is tiny evenly, performance boost.On the other hand, microwave sintering has the feature of selectivity heating, that is: absorb when the different material of microwave ability heat in given microwave field and will obtain different heats, thisly because the different microwave heating behavior of material is called as selectivity, heats.
For metal-powder, can be drawn by classical Maxwell equation: the ability that metal-powder absorbs microwave raises along with temperature and strengthens.Therefore, by the particular design to microwave sintering insulation construction and microwave sintering process, make goods subregion temperature higher, because metal-powder under high temperature can be more effectively by microwave heating, should in the whole sintering stage, just can remain comparatively high temps in zone so, and then in goods, keep significant thermograde in the whole sintering stage.Like this, at the sintering of same goods inside gradient temperature, cause shrinking, the difference of hole, can form the alloy (distribution gradient that comprises hole quantity, pore size, grain size, alloying constituent) of gradient-structure, therefore, it is feasible that microwave sintering prepares the gradient-porosity alloy.
The present invention is owing to adopting above-mentioned insulation construction and sintering process, in the incubation cavity structure, and the thinner adiabator layer of an end setting, and adopt the method in this end perforate to increase thermolysis; The pressed compact that makes to be in this end is in lower state of temperature all the time when microwave heating; And, at the thicker adiabator layer of the other end setting, strengthen heat insulation effect; Simultaneously, at this end, the boosting material is set, strengthens the ability that this end absorbs microwave; Make the pressed compact of this end be in all the time higher state of temperature, thereby form significant thermograde in pressed compact; The existence of thermograde, the difference of contraction, hole while causing sintering, the alloy (distribution gradient that comprises hole quantity, pore size, grain size, alloying constituent) of formation gradient-structure.
By changing two ends lagging material layer thickness and the boosting material amount of inserting, all can play the effect of controlling temperature gradient distribution.
In addition, the present invention in the microwave sintering process, low thermophase (<0.7Ts, Ts are sintering temperature) adopt lower heat-up rate (5 ℃/min).Low thermophase adopts lower heat-up rate can improve sintered body intensity, the thermal shocking of avoiding next higher heat-up rate and thermograde to bring, to keep green body quality, hot stage (0.7Ts-Ts) adopt faster heat-up rate (>20 ℃/min), by controlling microwave output power, can realize the adjusting of thermograde;
Advantage and the positively effect of invention:
The present invention adopts Microwave Sintering Techniques to produce the gradient-structure alloy, can in common industrial microwave High Temperature Furnaces Heating Apparatus, prepare the gradient-porosity alloy material by sintering; After obtaining the gradient-porosity alloy, can utilize again the alloy material of existing infiltration process prepared composition gradient, whole technological process is easy to design, simply controlled, has reduced cost, and wide prospect is arranged.With traditional technology, compare, the present invention need to not make the base substrate of gradient-structure before sintering, but adopts the microwave selective heating technique to form the gradient temperature field, controls the sintering effect of goods different zones, obtains controlled gradient structure structure.Can be used for industrial production.
The accompanying drawing explanation
The insulation construction master sectional view of accompanying drawing 1 for using in the embodiment of the present invention.
Accompanying drawing 2 is the A-A sectional view of accompanying drawing 1.
In figure: 1-thermal insulation layer, 2-sintering cavity, 3-louvre, 4-goods, 5-boosting material.
Embodiment
1. purity is greater than to 99.5%, the W powder of mean particle size 1.98 μ m is with ratio of grinding media to material 1: 1, rotating speed 150rpm, ball milling 6h in the Stainless Steel Ball mill tube, be pressed into pressed compact after taking-up;
2. use sapphire whisker as thermal insulator, in thermal insulator, add SiC as the boosting material, as shown in the figure, the boosting material SiC amount of putting into is 300g to insulation construction.
3. pressed compact is positioned in sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump by Bas Discharged in micro-wave oven furnace chamber, then pass into N
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 1000 ℃ with the heat-up rate of 5 ℃/min, then regulate microwave input power, make heat-up rate reach 25 ℃/min, temperature reaches 1450 ℃, closes microwave source, cooling rear taking-up goods;
The goods one end porosity obtained is about 25%, and the other end is about 35%.After this W base was placed in Cu liquation infiltration, can obtain an end composition was W-15Cu, and an end is the alloy that the component gradient of W-25Cu distributes.
1. purity is greater than to 99.5%, the W powder of mean particle size 1.98 μ m, purity is greater than 99.5%, the Cu powder of mean particle size 9 μ m, purity is greater than 99.5%, the Ni powder of mean particle size 2.3 μ m, press 95W-4Cu-1Ni mass percent batching, with ratio of grinding media to material 1: 1, rotating speed 150rpm, ball milling 6h in the Stainless Steel Ball mill tube, be pressed into pressed compact after taking-up;
2. use sapphire whisker as thermal insulator, in thermal insulator, add SiC as the boosting material, as shown in the figure, the boosting material SiC amount of putting into is 300g to insulation construction.
3. pressed compact is positioned in sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump by Bas Discharged in micro-wave oven furnace chamber, then pass into N
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 1000 ℃ with the heat-up rate of 5 ℃/min, then regulate microwave input power, make heat-up rate reach 25 ℃/min, temperature reaches 1400 ℃, closes microwave source, cooling rear taking-up goods;
The goods one end porosity obtained is about 20%, and the other end is about 40%.After this W base was placed in Cu liquation infiltration, can obtain an end composition was W-25Cu, and W crystal grain is about 10 μ m; The other end is the alloy that the component gradient of W-35Cu distributes, and W crystal grain is about 2 μ m.
1. purity is greater than to 99.5%, the W powder of mean particle size 1.98 μ m, purity is greater than 99.5%, the Ni powder of mean particle size 2.3 μ m, purity is greater than 99.5%, the Fe powder of mean particle size 2.3 μ m, press 90W-7Ni-3Fe mass percent batching, with ratio of grinding media to material 1: 1, rotating speed 150rpm, in the Stainless Steel Ball mill tube, mix 6h, after taking-up, be pressed into pressed compact;
2. use sapphire whisker as thermal insulator, in thermal insulator, add SiC as the boosting material, as shown in the figure, the boosting material SiC amount of putting into is 300g to insulation construction.
3. pressed compact is positioned in sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump by Bas Discharged in micro-wave oven furnace chamber, then pass into H
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 1000 ℃ with the heat-up rate of 5 ℃/min, then regulate microwave input power, make heat-up rate reach 25 ℃/min, temperature reaches 1500 ℃, closes microwave source, cooling rear taking-up goods;
The goods one end W crystal grain obtained is about 12 μ m, and tensile strength is 900MPa, unit elongation 15%; The other end W crystal grain is about 4 μ m, and tensile strength is 700MPa, unit elongation 5%.
1. purity is greater than to 99.5%, the Cu powder of mean particle size 9 μ m, with ratio of grinding media to material 1: 1, rotating speed 150rpm, ball milling 6h in the Stainless Steel Ball mill tube, be pressed into pressed compact after taking-up;
2. use sapphire whisker as thermal insulator, in thermal insulator, add SiC as the boosting material, as shown in the figure, the boosting material SiC amount of putting into is 100g to insulation construction.
3. pressed compact is positioned in sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump by Bas Discharged in micro-wave oven furnace chamber, then pass into N
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 650 ℃ with the heat-up rate of 5 ℃/min, then regulate microwave input power, make heat-up rate reach 25 ℃/min, temperature reaches 960 ℃, closes microwave source, cooling rear taking-up goods;
The goods one end porosity obtained is 3%; The other end porosity is about 30%.
Claims (4)
1. a microwave sintering prepares the method for porosity gradient metal or alloy material, comprises the steps:
The first step: base
Porosity gradient alloy compositions proportioning according to design, take each component, and powder metallurgy blank-making technology batch mixing, compression moulding, obtain pressed compact routinely;
Second step: pressed compact parcel
The pressed compact that the first step is obtained is placed in the incubation cavity of being made by lagging material, and wall thickness one end of described incubation cavity is thin, and an end is thick; The end that described incubation cavity is thin is provided with the heat radiation through hole; The end that described incubation cavity is thick is placed with the boosting material, and the fusing point of described boosting material is higher 200 ℃ than sintering temperature;
The 3rd step: sintering
The pressed compact that second step is wrapped is placed in the industrial microwave High Temperature Furnaces Heating Apparatus, regulates microwave output power, and the control pressed compact is warming up to 0.7 times of sintering temperature Ts with the speed of 5-10 ℃/min; Then, be warming up to sintering temperature with 20-50 ℃/min, close microwave source, furnace cooling.
2. a kind of microwave sintering according to claim 1 prepares the method for porosity gradient metal or alloy material, it is characterized in that: described boosting material is SiC.
3. a kind of microwave sintering according to claim 2 prepares the method for porosity gradient metal or alloy material, it is characterized in that: described lagging material is aluminum oxide lagging material or alumina-mullite lagging material.
4. according to the described a kind of microwave sintering of claim 1-3 any one, prepare the method for porosity gradient metal or alloy material, it is characterized in that: described alloy is selected from a kind of in W, Fe, Cu, Ti, Al, Mo alloy.
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| CN107740193B (en) * | 2017-10-12 | 2020-07-31 | 钢铁研究总院 | Gradient temperature field multichannel honeycomb array crucible |
| CN108213421A (en) * | 2017-12-15 | 2018-06-29 | 昆明理工大学 | A kind of method that microwave thermal decomposition prepares titanium-aluminum alloy material |
| CN115637364B (en) * | 2022-09-07 | 2023-08-25 | 合肥工业大学 | W-Cu continuous gradient composite material and preparation method thereof |
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| Title |
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| 周承商等.W-Ni-Fe高密度合金的微波烧结.《中国有色金属学报》.2009,第19卷(第9期),第1601-1607页. * |
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