CN102363844A - 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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- CN102363844A CN102363844A CN2011103407957A CN201110340795A CN102363844A CN 102363844 A CN102363844 A CN 102363844A CN 2011103407957 A CN2011103407957 A CN 2011103407957A CN 201110340795 A CN201110340795 A CN 201110340795A CN 102363844 A CN102363844 A CN 102363844A
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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.Be meant a kind of method that adopts the microwave sintering technology to prepare gradient-porosity metal or alloy material especially.Belong to microwave application and porosity gradient alloy preparing technical field.
Background technology
The technology of preparing of prior function gradient material mainly contains plasma spraying, electrophoretic deposition, vapour deposition, spreads methods such as synthetic, laser sintered certainly.There are shortcomings such as complex process, equipment requirements height, cost height in these methods.
The principle of microwave sintering technology is micro-wave energy is converted into 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 report such as the Roy of Pennsylvania State Univ-Univ Park USA in 1999 microwave sintering iron-based powder metallurgy parts proves metal-powder ability quilt microwave sintering effectively.
Present research is thought, because 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 to obtain different heats, thisly heats because of the different microwave heating behavior of material is called as selectivity.
For metal-powder, can be drawn by classical Maxwell equation: the ability of metal-powder absorption microwave raises along with temperature and strengthens.That is to say that 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, do not appear in the newspapers so far.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and provide a kind of process 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.Through the microwave sintering insulation construction and the microwave sintering process of particular design, in sintering process, form controlled thermograde, the difference of contraction, hole when utilizing thermograde to cause the alloy material sintering forms 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 takes by weighing each component, by conventional powder metallurgy blank-making technology batch mixing, compression moulding, obtains pressed compact;
Second step: pressed compact parcel
The pressed compact that the first step is obtained places the incubation cavity of being processed by lagging material, and wall thickness one end of said incubation cavity is thin, and an end is thick;
The 3rd step: sintering
The good pressed compact of the second step parcel is placed the industrial microwave High Temperature Furnaces Heating Apparatus, regulate microwave output power, 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, close microwave source, furnace cooling with 20-50 ℃/min.
A kind of microwave sintering of the present invention prepares in the method for porosity gradient metal or alloy material, and the end that said incubation cavity is thin is provided with the heat radiation through hole.
A kind of microwave sintering of the present invention prepares in the method for porosity gradient metal or alloy material, and the end that said incubation cavity is thick is placed with the boosting material, and the fusing point of said boosting material is higher 200 ℃ than sintering temperature.
A kind of microwave sintering of the present invention prepares in the method for porosity gradient metal or alloy material, and said boosting material is SiC.
A kind of microwave sintering of the present invention prepares in the method for porosity gradient metal or alloy material, and said lagging material is aluminum oxide lagging material or alumina-mullite lagging material.
A kind of microwave sintering of the present invention prepares in the method for porosity gradient metal or alloy material, and said alloy is selected from a kind of in W, Fe, Cu, Ti, Al, the Mo alloy.
Mechanism of the present invention is sketched in following: research is thought, because the volume effect of microwave heating can make tiny even, the performance boost of material structure.On the other hand, microwave sintering has the characteristic of selectivity heating, that is: absorb when the different material of microwave ability heat in given microwave field to obtain different heats, thisly heats because of the different microwave heating behavior of material is called as selectivity.
For metal-powder, can be drawn by classical Maxwell equation: the ability of metal-powder absorption microwave raises along with temperature and strengthens.Therefore; Through particular design to microwave sintering insulation construction and microwave sintering process; Make goods subregion temperature higher; Because metal-powder can should just can remain comparatively high temps in the whole sintering stage in the zone, and then in goods, keep significant thermograde in the whole sintering stage more effectively by microwave heating so under the high temperature.Like this; Cause shrinking at the sintering of same goods inside gradient temperature, 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 adopt above-mentioned insulation construction and sintering process, in the incubation cavity structure, and the adiabator layer that an end setting is thin, and the method that is employed in this end perforate increases thermolysis; Make the pressed compact that is in this end when microwave heating, be in lower state of temperature all the time; And, strengthen heat insulation effect at the thicker adiabator layer of the other end setting; Simultaneously, the boosting material is set, strengthens the ability that this end absorbs microwave at this end; Make the pressed compact of this end be in higher state of temperature all the time, thereby in pressed compact, form significant thermograde; The existence of thermograde, the difference of contraction, hole when causing sintering, the alloy (distribution gradient that comprises hole quantity, pore size, grain size, alloying constituent) of formation gradient-structure.
Through changing the effect that two ends lagging material layer thickness and the boosting material amount of inserting all can play the controlled 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; Adopt faster (＞20 ℃/min),, can realize the adjusting of thermograde of heat-up rates at hot stage (0.7Ts-Ts) through the controlled microwave output rating;
The advantage and the positively effect of invention:
The present invention adopts the microwave sintering technology 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 the alloy material of existing infiltration process prepared composition gradient again, whole technological process is easy to design, and simple controllable has reduced cost, and wide prospect is arranged.Compare with traditional technology, the present invention need not make the base substrate of gradient-structure before sintering, but adopts the microwave selective heating technique to form the gradient temperature field, and the sintering effect of control goods different zones obtains controlled gradient structure structure.Can be used for industrial production.
Description of drawings
The insulation construction master sectional view of accompanying drawing 1 for using in the embodiment of the invention.
Accompanying drawing 2 is the A-A sectional view of accompanying drawing 1.
Among the figure: 1-thermal insulation layer, 2-sintering cavity, 3-louvre, 4-goods, 5-boosting material.
Embodiment
1. with purity greater than 99.5%, the W powder of mean particle size 1.98 μ m is with ball-to-powder weight ratio 1: 1, rotating speed 150rpm, ball milling 6h in the Stainless Steel Ball mill tube is pressed into pressed compact after the taking-up;
2. use sapphire whisker as thermal insulator, add SiC in the thermal insulator as the boosting material, insulation construction is as shown in the figure, and the boosting material SiC amount of putting into is 300g.
3. pressed compact is positioned in the sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump air in the micro-wave oven furnace chamber is discharged, feed N then
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 1000 ℃ with the heat-up rate of 5 ℃/min, regulate microwave input power then, make heat-up rate reach 25 ℃/min, temperature reaches 1450 ℃, closes microwave source, and goods are taken out in the cooling back;
The goods one end porosity that obtains is about 25%, and the other end is about 35%.After this W base placed 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. with purity greater than 99.5%, the W powder of mean particle size 1.98 μ m; Purity greater than 99.5%, the Cu powder of mean particle size 9 μ m; Purity greater than 99.5%, the Ni powder of mean particle size 2.3 μ m, press 95W-4Cu-1Ni mass percent batching, with ball-to-powder weight ratio 1: 1, rotating speed 150rpm; Ball milling 6h in the Stainless Steel Ball mill tube is pressed into pressed compact after the taking-up;
2. use sapphire whisker as thermal insulator, add SiC in the thermal insulator as the boosting material, insulation construction is as shown in the figure, and the boosting material SiC amount of putting into is 300g.
3. pressed compact is positioned in the sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump air in the micro-wave oven furnace chamber is discharged, feed N then
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 1000 ℃ with the heat-up rate of 5 ℃/min, regulate microwave input power then, make heat-up rate reach 25 ℃/min, temperature reaches 1400 ℃, closes microwave source, and goods are taken out in the cooling back;
The goods one end porosity that obtains is about 20%, and the other end is about 40%.After this W base placed 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. with purity greater than 99.5%, the W powder of mean particle size 1.98 μ m; Purity greater than 99.5%, the Ni powder of mean particle size 2.3 μ m; Purity greater than 99.5%, the Fe powder of mean particle size 2.3 μ m, press 90W-7Ni-3Fe mass percent batching, with ball-to-powder weight ratio 1: 1, rotating speed 150rpm; In the Stainless Steel Ball mill tube, mix 6h, be pressed into pressed compact after the taking-up;
2. use sapphire whisker as thermal insulator, add SiC in the thermal insulator as the boosting material, insulation construction is as shown in the figure, and the boosting material SiC amount of putting into is 300g.
3. pressed compact is positioned in the sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump air in the micro-wave oven furnace chamber is discharged, feed H then
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 1000 ℃ with the heat-up rate of 5 ℃/min, regulate microwave input power then, make heat-up rate reach 25 ℃/min, temperature reaches 1500 ℃, closes microwave source, and goods are taken out in the cooling back;
The goods one end W crystal grain that obtains 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. with purity greater than 99.5%, the Cu powder of mean particle size 9 μ m, with ball-to-powder weight ratio 1: 1, rotating speed 150rpm, ball milling 6h in the Stainless Steel Ball mill tube is pressed into pressed compact after the taking-up;
2. use sapphire whisker as thermal insulator, add SiC in the thermal insulator as the boosting material, insulation construction is as shown in the figure, and the boosting material SiC amount of putting into is 100g.
3. pressed compact is positioned in the sintering cavity, puts into the microwave high-temperature stove;
4. with vacuum pump air in the micro-wave oven furnace chamber is discharged, feed N then
2Atmosphere protection; Regulate microwave high-temperature stove output rating, be heated to 650 ℃ with the heat-up rate of 5 ℃/min, regulate microwave input power then, make heat-up rate reach 25 ℃/min, temperature reaches 960 ℃, closes microwave source, and goods are taken out in the cooling back;
The goods one end porosity that obtains is 3%; The other end porosity is about 30%.
Claims (6)
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 takes by weighing each component, by conventional powder metallurgy blank-making technology batch mixing, compression moulding, obtains pressed compact;
Second step: pressed compact parcel
The pressed compact that the first step is obtained places the incubation cavity of being processed by lagging material, and wall thickness one end of said incubation cavity is thin, and an end is thick;
The 3rd step: sintering
The good pressed compact of the second step parcel is placed the industrial microwave High Temperature Furnaces Heating Apparatus, regulate microwave output power, 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, close microwave source, furnace cooling with 20-50 ℃/min.
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: the end that said incubation cavity is thin is provided with the heat radiation through hole.
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: the end that said incubation cavity is thick is placed with the boosting material, and the fusing point of said boosting material is higher 200 ℃ than sintering temperature.
4. a kind of microwave sintering according to claim 3 prepares the method for porosity gradient metal or alloy material, it is characterized in that: said boosting material is SiC.
5. a kind of microwave sintering according to claim 4 prepares the method for porosity gradient metal or alloy material, it is characterized in that: said lagging material is aluminum oxide lagging material or alumina-mullite lagging material.
6. prepare the method for porosity gradient metal or alloy material according to any described a kind of microwave sintering of claim 1-5, it is characterized in that: said alloy is selected from a kind of in W, Fe, Cu, Ti, Al, the Mo alloy.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925757A (en) * | 2012-10-10 | 2013-02-13 | 上海大学 | Method for preparing Al-Fe alloy by virtue of nanometre powder |
| CN107740193A (en) * | 2017-10-12 | 2018-02-27 | 钢铁研究总院 | A kind of 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 |
| CN115637364A (en) * | 2022-09-07 | 2023-01-24 | 合肥工业大学 | W-Cu continuous gradient composite material and preparation method thereof |
Citations (1)
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| CN102199717A (en) * | 2011-04-15 | 2011-09-28 | 北京理工大学 | Gradient multiferroic material and preparation method thereof |
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| CN102199717A (en) * | 2011-04-15 | 2011-09-28 | 北京理工大学 | Gradient multiferroic material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 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》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925757A (en) * | 2012-10-10 | 2013-02-13 | 上海大学 | Method for preparing Al-Fe alloy by virtue of nanometre powder |
| CN102925757B (en) * | 2012-10-10 | 2014-12-03 | 上海大学 | Method for preparing Al-Fe alloy by virtue of nanometre powder |
| CN107740193A (en) * | 2017-10-12 | 2018-02-27 | 钢铁研究总院 | A kind of gradient temperature field multichannel honeycomb array crucible |
| 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 |
| CN115637364A (en) * | 2022-09-07 | 2023-01-24 | 合肥工业大学 | W-Cu continuous gradient composite material and preparation method thereof |
| 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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