CN111687409A - Near net forming method and subsequent sintering process for titanium and titanium alloy - Google Patents
Near net forming method and subsequent sintering process for titanium and titanium alloy Download PDFInfo
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- CN111687409A CN111687409A CN201910186205.6A CN201910186205A CN111687409A CN 111687409 A CN111687409 A CN 111687409A CN 201910186205 A CN201910186205 A CN 201910186205A CN 111687409 A CN111687409 A CN 111687409A
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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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
- B22F3/101—Changing atmosphere
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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Abstract
A titanium and titanium alloy near net forming method and a subsequent sintering process. The invention relates to a method for realizing powder near-net forming by utilizing hydrogen absorption expansion of titanium alloy powder. Putting titanium powder or titanium alloy powder A or titanium-containing mixed powder B into a rigid die, wherein the inner cavity of the die is designed according to the geometric shape of a product; putting the blank body into a sintering furnace, and introducing hydrogen to enable the titanium alloy powder to absorb hydrogen; the volume expansion effect of hydrogen absorption of the titanium alloy powder enables the powder to be mutually extruded, so that a powder blank with higher strength is obtained; then dehydrogenating the blank and the die in a vacuum environment, and conveniently taking out the powder blank after dehydrogenation; and finally sintering the powder blank to obtain a finished product with a target shape. The invention provides a novel near-net forming method for titanium alloy powder metallurgy. The method can obtain products with complex shapes, is suitable for various titanium powder and titanium alloy powder with poor pressing performance, and the powder blank and the sintered finished product obtained by the method have high density, good uniformity and improved performance.
Description
Technical Field
The invention relates to a method for near-net forming of titanium alloy powder; in particular to a method for promoting powder near-net forming by utilizing hydrogen absorption expansion of titanium alloy powder.
Background
The titanium alloy and the titanium-based composite material have wide application in the fields of aviation, aerospace, ships, weapons, nuclear energy, biomedical use and the like due to the advantages of low density, high specific strength, corrosion resistance, good medium-temperature performance, no magnetism, good biocompatibility and the like, and are important metal materials. There are various methods for preparing titanium alloy, including precision casting, machining, additive manufacturing, and powder metallurgy, but the high cost of titanium limits its wide application.
The titanium alloy and the titanium-based composite material have the problems of high processing difficulty and high processing cost, so that the application of the final product is limited. The powder metallurgy forming technology can prepare the near-net-shaped titanium alloy parts with accurate size and less processing amount. The forming method mainly comprises cold pressing, cold isostatic pressing, hot isostatic pressing and injection forming. However, titanium alloy powder has poor pressing performance and difficult molding, and is easy to generate defects in subsequent sintering, and has low density and mechanical properties.
The forming technologies such as powder hot isostatic pressing, hot pressing sintering, spark plasma sintering and the like can manufacture materials with good performance, but the special processes have high cost, large popularization difficulty and great limitation on the size of products.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a process for promoting the near net shape forming and the subsequent sintering of the powder by utilizing the hydrogen absorption expansion of the titanium alloy powder for the first time.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; putting titanium powder or titanium alloy powder A or titanium-containing mixed powder B into a rigid die to obtain a component C; putting the assembly into a hydrogen furnace, heating and introducing hydrogen to enable the titanium alloy powder or the titanium-containing mixed powder to absorb hydrogen; the volume expansion effect of the titanium alloy powder or the titanium-containing mixed powder is utilized to enable the titanium alloy powder or the titanium-containing mixed powder to be mutually extruded to obtain a powder blank body with higher strength; then dehydrogenating the powder blank under vacuum or inert atmosphere, and taking out the powder blank D after dehydrogenation; and finally, sintering the powder blank D at high temperature to obtain a finished product with a target shape. The temperature of the high-temperature sintering is higher than the temperature of hydrogen absorption.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the hydrogen absorption process is controlled as follows: heating the component C, and introducing hydrogen; preserving heat, then cooling, continuously introducing hydrogen, and finishing; the hydrogen absorption volume expansion of the titanium and titanium alloy powder in the hydrogen absorption process must achieve the effect of plastic deformation so that the powder blank has good bonding strength.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the dehydrogenation process is controlled as follows: heating the component C to a certain temperature in vacuum or flowing inert atmosphere (including argon), and preserving the temperature, and finishing; in the dehydrogenation process, the titanium and titanium alloy powder blank must have a certain degree of volume shrinkage so as to achieve the effect that the powder blank D can be smoothly demoulded.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the high-temperature sintering process is controlled as follows: placing the powder green body D in a sintering furnace, heating to a sintering temperature, preserving heat, cooling, and finishing; the high-temperature sintering temperature is 1000-1300 ℃, and during sintering, the vacuum degree in the furnace is lower than 10-3Pa. During sintering, the powder body must be made to have a high degree of compactness in order to obtain good mechanical properties.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process;
the chemical composition of the titanium powder is pure titanium,
the titanium alloy powder A is a titanium alloy containing more than 40 mol percent of titanium element,
the average particle size of the titanium powder and the titanium alloy powder A is less than 200 microns;
the titanium powder and the titanium alloy powder have hydrogen absorption capacity, and the titanium powder and the titanium alloy powder have hydrogen absorption expansion effect.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process;
the titanium-containing mixed powder B contains titanium or titanium alloy powder with hydrogen absorption expansion capability; the average particle size of the titanium powder in the titanium-containing mixed powder B is less than 200 microns.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; in the titanium-containing mixed powder B, the titanium powder and/or the titanium alloy powder accounts for more than 50% of the total mass of the mixed powder. In industrial applications, the residual powder can be other metal powder, or ceramic phase reinforced particles, or reinforced fiber material, etc.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the powder blank D obtained after the hydrogen absorption process is finished has certain strength and higher density and can be designed into a complex shape.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; filling the inner cavity of the die with titanium powder or titanium alloy powder A or titanium-containing mixed powder B; packaging, fastening and reserving a ventilation gap, wherein the leakage of powder cannot be caused by the gap; resulting in component C.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; all parts of the packaged die are kept fastened and cannot loosen in the processes of hydrogen absorption and dehydrogenation.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the material of the mould does not react with hydrogen and can be repeatedly used.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the inner cavity of the die can be designed into a finally formed geometric shape, and the die can be conveniently detached after the dehydrogenation process;
the invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the hydrogen absorption temperature range is 400-800 ℃, preferably 600-700 ℃, and the hydrogen partial pressure is 5-100%.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the dehydrogenation temperature is 600-800 ℃, preferably 700-800 ℃, and the vacuum degree of vacuum annealing is less than 10-3Pa。
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; after the dehydrogenation is finished, vacuum sintering is carried out in a vacuum sintering furnace, the sintering temperature range is 1000-1300 ℃, the preferred range is 1100-1250 ℃, and the vacuum degree is lower than 10-3Pa。
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; directly loading titanium alloy powder into a rigid die to obtain a pretreatment assembly; introducing hydrogen into the pretreatment assembly to enable the titanium alloy powder to absorb hydrogen; extruding the titanium alloy powder by utilizing the volume expansion effect of the titanium alloy powder to obtain a blank; then dehydrogenating under a vacuum environment; finally, sintering is carried out to densify and form the titanium alloy powder in a near net shape;
the hydrogen absorption process is controlled as follows: firstly, heating a pretreatment component C to a temperature of H1 in an inert atmosphere or vacuum, then introducing hydrogen, preserving heat, then cooling to a temperature of H2, and preserving heat, wherein the value range of H1 is 500-900 ℃;
or
The hydrogen absorption process is controlled as follows: firstly, heating a pretreatment component C to a temperature H3 in an inert atmosphere or vacuum, then introducing hydrogen, preserving heat, continuously heating to H1, and continuously introducing hydrogen; preserving heat; then, cooling to a temperature H2, continuously introducing hydrogen, and preserving heat, wherein the value range of H1 is 500-900 ℃; the H3 is less than H1.
More preferably, the titanium alloy powder is Ti6Al 4V. The pretreatment component C is a sample with a mold.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the holding time of H1 is less than or equal to 24 hours, preferably 1-12 hours;
after the temperature is kept at H1, the temperature is reduced to H2 at the cooling speed of 0.1-20 ℃/min; the incubation time at H2 is 24 hours or less, preferably 2 to 18 hours.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the inert atmosphere is argon atmosphere, the rate of cooling from H1 to H2 is 0.1-5 ℃/min, and the range of H1 is 750-900 ℃; the range of H2 is 600-700 ℃; the H2 is less than H1.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; after the hydrogen absorption is finished, the heat preservation vacuum annealing is carried out at the dehydrogenation temperature D, the range of the dehydrogenation temperature D is 700-800 ℃, and the vacuum degree of the vacuum annealing is lower than 10-3Pa。
The invention relates to titanium and titanium alloyA near net shape forming method and a subsequent sintering process; after the dehydrogenation is finished, vacuum sintering is carried out in a vacuum sintering furnace, the sintering temperature T4 ranges from 1000 ℃ to 1300 ℃, and the vacuum degree is lower than 10-3Pa。
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; the material of the mold is preferably: at least one of heat-resistant steel, high-temperature-resistant stainless steel, high-temperature alloy and high-temperature ceramic.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; after the titanium alloy powder absorbs hydrogen, the absorbed hydrogen can be completely removed by heating to raise the temperature or reducing the hydrogen partial pressure.
The invention relates to a titanium and titanium alloy near net forming method and a subsequent sintering process; in industrial applications, the article may be, but is not limited to: near-net shaping of titanium alloy powder; near net shape of other hydrogen absorbing powders.
Principles and advantages
The invention provides a method for promoting powder near-net-shape forming by utilizing the synergistic effect of hydrogen absorption expansion and a rigid die of titanium and titanium alloy powder in a hydrogen environment.
The titanium and titanium alloy powder of the present invention absorbs hydrogen to expand in a hydrogen atmosphere, so that expansion stress is applied to the titanium alloy powder itself. Meanwhile, under the condition that the volume of a closed space (a rigid mold cavity) is unchanged or the volume change is smaller than the hydrogen absorption expansion volume, the rigid mold can restrain materials, so that the materials are mutually extruded, and the powder is pressed into a blank with certain strength; then heating and dehydrogenating in a vacuum or inert gas environment, wherein hydrogen in the embryo body overflows to shrink and separate from the inner wall of the cavity; and finally sintering in vacuum or inert gas environment.
Compared with the traditional powder metallurgy densification forming technology or metal plastic processing technology, the method has the following advantages:
(1) near net shape, rigid moulds of various geometric shapes can be designed according to requirements, and the powder is directly used for finished parts. When the structural requirement of the product is complex and the requirement on the dimensional accuracy is higher, the advantages are particularly obvious compared with the traditional powder forming technology.
(2) The production equipment and the die are simple, the production period is short, the operation is simple, the production cost is low, and the efficiency is high.
(3) Compared with the traditional powder forming treatment temperature, the treatment temperature of the process is lower, and the product has higher density, good strength and mechanical property and obvious performance advantage.
Drawings
Figure 1 shows a schematic view of a rigid mold.
Fig. 2 is a stainless steel mold.
It can be seen from fig. 1 that by changing the geometry of the constraining blocks 2, the internal structure of the rigid mold can be designed adjustably.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the present invention, the mold after encapsulation; in the heating process, the condition that the parts are loosened and fall off cannot occur.
The first embodiment is as follows:
1. titanium alloy powder (Ti6Al4V powder, purity 99%) is put into a stainless steel die with a cylindrical inner cavity (diameter 50mm, height 100mm), the powder is uniformly filled in the die, and the die is packaged and fastened.
2. Placing the assembled mould into a sintering furnace, heating to 800 ℃ under the argon atmosphere, and preserving heat for one hour; introducing hydrogen (hydrogen flow is 1L/min), cooling to 650 ℃ at the speed of 1 ℃/min, keeping introducing the hydrogen, keeping the temperature for 4 hours, and cooling the furnace.
3. Turning to a vacuum sintering furnace, and vacuumizing (vacuum degree is less than 10)-3Pa), raising the temperature to 750 ℃, keeping the temperature for 4 hours, and then blowing out the furnace for cooling.
4. Opening the vacuum sintering furnace, taking out and opening the mold, continuously putting the sample into the vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 1250 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
5. And opening the vacuum sintering furnace, and taking out to obtain a formed cylindrical sample.
Example two:
1. titanium alloy powder (Ti6Al4V powder, purity 99%) is put into a stainless steel die with the shape shown in figure 2, the titanium alloy powder is uniformly filled in the die, and the die is packaged and fastened.
2. Placing the assembled mould into an atmosphere sintering furnace, heating to 800 ℃ under the argon atmosphere, and preserving heat for one hour; introducing hydrogen (hydrogen flow is 1L/min), cooling to 650 ℃ at the speed of 1 ℃/min, keeping introducing the hydrogen, keeping the temperature for 4 hours, and cooling the furnace.
3. Turning to a vacuum sintering furnace, and vacuumizing (vacuum degree is less than 10)-3Pa), raising the temperature to 750 ℃, keeping the temperature for 4 hours, and then blowing out the furnace for cooling.
4. Opening the vacuum sintering furnace, taking out and opening the mold, continuously putting the sample into the vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 1250 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
5. And opening the vacuum sintering furnace, and taking out to obtain a molded bolt-shaped sample.
Example three:
1. titanium powder (purity 99%) is put into a stainless steel mold with an inner cavity of 50X 50mm, the mold is uniformly filled, and the mold is packaged and fastened.
2. Placing the assembled mould into an atmosphere sintering furnace, heating to 800 ℃ under the argon atmosphere, and preserving heat for one hour; introducing hydrogen (hydrogen flow is 1L/min), cooling to 600 ℃ at the speed of 1 ℃/min, keeping introducing the hydrogen, keeping the temperature for 4 hours, and cooling the furnace.
3. Turning to a vacuum sintering furnace, and vacuumizing (vacuum degree is less than 10)-3Pa), raising the temperature to 750 ℃, keeping the temperature for 4 hours, and then blowing out the furnace for cooling.
4. Opening the vacuum sintering furnace, taking out and opening the mold, continuously putting the sample into the vacuum sintering furnace, and vacuumizing (the vacuum degree is less than 10)-3Pa), raising the temperature to 1250 ℃, keeping the temperature for 2 hours, and then blowing out the furnace for cooling.
5. And opening the vacuum sintering furnace, and taking out to obtain a molded titanium block sample.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. A titanium and titanium alloy near net forming method and a subsequent sintering process; the method is characterized in that: putting titanium powder or titanium alloy powder A or titanium-containing mixed powder B into a rigid die to obtain a component C; putting the assembly into a hydrogen furnace, heating and introducing hydrogen to ensure that the titanium powder or the titanium alloy powder or the titanium-containing mixed powder absorbs hydrogen; the method comprises the following steps of (1) mutually extruding titanium alloy powder or titanium-containing mixed powder by utilizing the hydrogen absorption volume expansion effect of the titanium powder or the titanium alloy powder or the titanium-containing mixed powder to obtain a powder blank D with higher strength; then dehydrogenating the powder blank under vacuum or inert atmosphere, and taking out the powder blank D after dehydrogenation; finally, sintering the powder blank D at high temperature to obtain a finished product with a target shape; the temperature of the high-temperature sintering is higher than the temperature of hydrogen absorption.
2. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that:
the hydrogen absorption process is controlled as follows: heating the component C, and introducing hydrogen; preserving heat, then cooling, continuously introducing hydrogen, and finishing; the hydrogen absorption volume expansion of the titanium and titanium alloy powder in the hydrogen absorption process must achieve the effect of plastic deformation to ensure that the powder blank has good bonding strength;
the dehydrogenation process is controlled as follows: heating the component C to a certain temperature in vacuum or flowing inert atmosphere, preserving the temperature, and finishing; in the dehydrogenation process, the titanium and titanium alloy powder blank must have certain volume shrinkage so as to achieve the effect that the powder blank D can be smoothly demoulded;
the high-temperature sintering process is controlled as follows: placing the powder green body D in a sintering furnace, heating to a sintering temperature, preserving heat, cooling, and finishing; the high-temperature sintering temperature is 1000-1300 ℃, and during sintering, the vacuum degree in the furnace is lower than 10-3Pa。
3. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that:
the chemical composition of the titanium powder is pure titanium,
the titanium alloy powder A is a titanium alloy containing more than 40 mol percent of titanium element,
the average particle size of the titanium powder and the titanium alloy powder A is less than 200 microns;
the titanium powder and the titanium alloy powder have hydrogen absorption capacity, and the titanium powder and the titanium alloy powder have hydrogen absorption expansion effect.
4. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that: the titanium-containing mixed powder B contains titanium or titanium alloy powder with hydrogen absorption expansion capability; the average particle size of the titanium powder in the titanium-containing mixed powder B is less than 200 microns.
5. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that: in the titanium-containing mixed powder B, the titanium powder and/or the titanium alloy powder accounts for more than 50% of the total mass of the mixed powder.
6. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that: filling the inner cavity of the die with titanium powder or titanium alloy powder A or titanium-containing mixed powder B; packaging, fastening and reserving a ventilation gap, wherein the leakage of powder cannot be caused by the gap; resulting in component C.
7. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that:
all parts of the packaged die are kept fastened and cannot loosen in the processes of hydrogen absorption and dehydrogenation;
the material of the mould does not react with hydrogen and can be repeatedly used.
8. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that: the inner cavity of the die can be designed into a finally formed geometric shape, and the die can be conveniently detached after the dehydrogenation process.
9. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that: the hydrogen absorption temperature is 400-800 ℃, and the hydrogen partial pressure is 5-100%.
10. The method for near net shape forming and subsequent sintering of titanium and titanium alloys of claim 1; the method is characterized in that: the dehydrogenation temperature is 600-800 ℃, and the vacuum degree of vacuum annealing is less than 10-3Pa。
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