CN113333753A - Sintering method of powder injection molding titanium alloy - Google Patents
Sintering method of powder injection molding titanium alloy Download PDFInfo
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- CN113333753A CN113333753A CN202110607459.8A CN202110607459A CN113333753A CN 113333753 A CN113333753 A CN 113333753A CN 202110607459 A CN202110607459 A CN 202110607459A CN 113333753 A CN113333753 A CN 113333753A
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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
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
- B22F3/1025—Removal of binder or filler not by heating 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
- B22F2201/11—Argon
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a sintering method of a powder injection molding titanium alloy, which comprises the following steps: putting the titanium alloy injection blank into a degreasing furnace, adding oxalic acid into the degreasing furnace, introducing argon, and degreasing at the degreasing temperature of 140 ℃ to obtain a degreased part; putting the degreased part into a high-vacuum metal furnace, introducing argon into the high-vacuum metal furnace, and heating the high-vacuum metal furnace to 600 ℃ from room temperature for negative pressure degreasing; then vacuum sintering is carried out, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 5 ℃/min, and the time lasts for 60 min; finally, continuously introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa, heating from 900 ℃ to 1200 ℃ at the speed of 3 ℃/min, and preserving the heat for 180 min; cooling to obtain the product. According to the invention, inert gas is used for protection in the degreasing and sintering processes, and the titanium alloy workpiece with high performance is obtained after sintering is finished through discontinuous vacuum and partial pressure sintering.
Description
Technical Field
The invention relates to the technical field of powder injection molding, in particular to a sintering method of a powder injection molding titanium alloy.
Background
The titanium alloy is an important metal developed in the middle of the 20 th century, and is widely applied to the fields of aerospace, automobiles, bioengineering (good compatibility), watches, sports goods, environmental protection and the like due to the excellent properties of low density, high specific strength, good corrosion resistance, high heat resistance, no magnetism, good welding performance and the like. However, titanium and titanium alloys have poor machinability and high manufacturing costs, which limits their industrial applications, especially in complex parts.
The Powder Injection Molding (PIM) technology is a product combining the traditional Powder metallurgy Molding technology and the plastic Injection Molding technology, has the advantages of few working procedures, no cutting or less cutting, high economic benefit and the like of the traditional Powder metallurgy technology, overcomes the characteristics of low material density, nonuniform material, low mechanical property, difficult thin wall forming and complex structural parts of the traditional Powder metallurgy technology, and particularly has advantages in the aspect of preparing near-net-shaped products with complex geometric shapes, uniform tissue structures and high performance.
However, titanium metal has high activity and is easily reacted with carbon, oxygen, nitrogen and the like to form TiC and TiO2And TiN and other compounds make the sintering density difficult to improve, thereby affecting the mechanical properties of products, and most of the titanium alloy products produced at present are low-strength products.
Disclosure of Invention
In order to solve the problems of the prior art, embodiments of the present invention provide a sintering method for powder injection molding a titanium alloy. The technical scheme is as follows:
in a first aspect, there is provided a sintering method of powder injection moulding a titanium alloy, the method comprising:
putting the titanium alloy injection blank into a degreasing furnace, adding oxalic acid into the degreasing furnace, introducing argon, and degreasing at the degreasing temperature of 140 ℃ to obtain a degreased part;
putting the degreased part into a high-vacuum metal furnace, introducing argon into the high-vacuum metal furnace, and heating the high-vacuum metal furnace from room temperature to 600 ℃ for negative pressure degreasing; then vacuum sintering is carried out, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 5 ℃/min, and the time lasts for 60 min; finally, continuously introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa, heating from 900 ℃ to 1200 ℃ at the speed of 3 ℃/min, and keeping the temperature for 180 min; cooling to obtain the product.
Further, the specific method for introducing argon into the high vacuum metal furnace and heating the high vacuum metal furnace from room temperature to 600 ℃ for negative pressure degreasing comprises the following steps:
introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, heating from room temperature to 250 ℃ at the heating rate of 2 ℃/min, and preserving heat for 120 min;
keeping the flow of argon unchanged, heating from 250 ℃ to 430 ℃ at a heating rate of 3 ℃/min, and keeping the temperature for 180 min;
keeping the flow of argon unchanged, heating from 430 ℃ to 600 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 240 min.
Further, the specific method of cooling is as follows:
introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa, cooling from 1200 ℃ to 600 ℃ at the speed of 3 ℃/min, and continuing air cooling until the temperature reaches the room temperature.
Further, the specific method for degreasing at the degreasing temperature of 140 ℃ by adding oxalic acid into a degreasing furnace and introducing argon gas into the furnace to obtain the degreased part comprises the following steps:
degreasing temperature 140 deg.C, adding oxalic acid into the degreasing furnace at a speed of 3g/min while maintaining the degreasing furnace at 2m3Introducing argon into the degreasing furnace at a speed of/h, and continuously degreasing for 1 h; then keeping the degreasing temperature, continuously adding oxalic acid into the degreasing furnace at the speed of 5g/min, and adding oxalic acid into the furnace at the speed of 3m3Introducing argon into the degreasing furnace at a speed of/h, and degreasing for 3 h; and cooling to obtain a degreased part.
Further, the method further comprises: placing the titanium alloy injection blank into a degreasing furnace, and then pouring the titanium alloy injection blank into the degreasing furnace at a height of 2m3Filling argon into the degreasing furnace at a flow rate of/h, and flushing the degreasing furnace and the titanium alloy injection molded blank for 1 hour.
Further, the method further comprises: defatting for 3 hr, and adding 1m3And introducing argon into the degreasing furnace at a speed of/h for 1h, and slowly cooling along with the furnace to obtain a degreased part.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: in the embodiment of the invention, a titanium alloy injection blank is placed into a degreasing furnace, oxalic acid is added into the degreasing furnace, argon is introduced into the degreasing furnace, and degreasing is carried out at a degreasing temperature of 140 ℃ to obtain a degreased part; putting the degreased part into a high-vacuum metal furnace, introducing argon into the high-vacuum metal furnace, and heating the high-vacuum metal furnace from room temperature to 600 ℃ for negative pressure degreasing; then vacuum sintering is carried out, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 5 ℃/min, and the time lasts for 60 min; finally, continuously introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa, heating from 900 ℃ to 1200 ℃ at the speed of 3 ℃/min, and keeping the temperature for 180 min; cooling to obtain the product. According to the invention, oxalic acid is adopted to carry out degreasing on the titanium alloy injection blank, inert gas is used for protection in the degreasing and sintering processes, no oxidation and no recarburization are ensured in the degreasing process, and alloy powder in the titanium alloy is prevented from reacting with oxygen/carbon through discontinuous vacuum and partial pressure sintering, so that a high-performance titanium alloy workpiece is obtained after sintering is completed.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
The embodiment of the invention provides a sintering method of a powder injection molding titanium alloy, which comprises the following steps:
putting the titanium alloy injection blank into a degreasing furnace for 2m3And filling argon into the degreasing furnace at a flow rate of/h, and flushing the degreasing furnace and the titanium alloy injection molded blank for 1 hour by using the argon to exhaust air in the degreasing furnace. Setting the degreasing temperature at 140 ℃, adding oxalic acid into a degreasing furnace at a speed of 3g/min and simultaneously adding oxalic acid at a speed of 2m to prevent surface peeling or chapping of the titanium alloy injection molded blank caused by over-fast degreasing3And introducing argon gas into the degreasing furnace at a flow rate of/h, and continuously degreasing for 1h to form a capillary channel on the surface of the workpiece. Keeping the degreasing temperature at 140 deg.C, continuously adding oxalic acid into the degreasing furnace at a speed of 5g/min, and increasing the flow of argon gas at 3m to completely take the formaldehyde decomposed by degreasing out of the degreasing furnace3Introducing argon into the degreasing furnace at a flow rate of/h, degreasing for 3h, and after reaching the standard degreasing rate (8.5 percent), performing degreasing at the rate of 1m3And introducing argon into the degreasing furnace for 1h at the flow rate of/h, and slowly cooling the titanium alloy injection blank along with the furnace to ensure that residual carbon which is not oxidized and decomposed into formaldehyde is not generated in the cooling process, thereby finally obtaining the degreased part.
And (3) putting the degreased part into a high-vacuum metal furnace, and firstly carrying out negative pressure degreasing to completely decompose the residual high-molecular binder in the degreased part.
The negative pressure degreasing is divided into three stages, and the specific treatment is as follows:
and introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, heating the high-vacuum metal furnace from room temperature to 250 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 120 min.
Keeping the flow of argon gas of 50L/min unchanged, heating from 250 ℃ to 430 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 180 min; the purpose of the prolonged holding time at this stage is to decompose the polymer material in this melting point range as completely as possible and carry it out by argon.
Keeping the flow of argon gas of 50L/min constant, heating from 430 ℃ to 600 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 240 min.
After the negative pressure degreasing is finished, discharging gas in the high vacuum metal furnace until the vacuum degree in the furnace reaches below 0.005Pa, then performing vacuum sintering, and raising the temperature from 600 ℃ to 900 ℃ at the speed of 5 ℃/min for 60 min. The residual trace carbon thermally decomposed can be completely isolated from the oxidation reaction with the metal in the degreased part by vacuum sintering.
And finally, carrying out partial pressure sintering, continuously introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa to effectively protect the titanium alloy from being oxidized in the high-temperature process, heating from 900 ℃ to 1200 ℃ at the speed of 3 ℃/min, and keeping the temperature for 180 min. The titanium alloy can be completely densified through partial pressure sintering, and the process is free of oxides and carbon residual dissolution.
After the partial pressure sintering is finished, in order to ensure that the titanium alloy is not oxidized in the cooling process, argon is continuously introduced into the high-vacuum metal furnace at the flow rate of 50L/min, the pressure of the argon is kept at 50KPa, the high-vacuum metal furnace is cooled to 600 ℃ from 1200 ℃ at the speed of 3 ℃/min, and then air cooling is started until the room temperature is reached.
The titanium alloy workpieces (example 1 and example 2) obtained by the above-described treatment were subjected to density, yield strength and ultimate tensile strength measurements, respectively, and the results are shown in table 1, in comparison with those obtained by the conventional sintering process (comparative example 1 and comparative example 2). As can be seen from Table 1, the titanium alloy workpiece treated by the method of the present invention has various properties superior to those of conventional sintering processes, and can meet the requirements of high-performance titanium alloy products.
TABLE 1 product parameters and Properties of the two Processes
| Detection group | Density g/cm3 | Yield strength MPa | Elongation (%) |
| Example 1 | 4.35 | 1020 | 11.6％ |
| Example 2 | 4.37 | 1050 | 11.8％ |
| Comparative example 1 | 4.26 | 956 | 8.8％ |
| Comparative example 2 | 4.28 | 962 | 9.3％ |
In the embodiment of the invention, a titanium alloy injection blank is placed into a degreasing furnace, oxalic acid is added into the degreasing furnace, argon is introduced into the degreasing furnace, and degreasing is carried out at a degreasing temperature of 140 ℃ to obtain a degreased part; putting the degreased part into a high-vacuum metal furnace, introducing argon into the high-vacuum metal furnace, and heating the high-vacuum metal furnace from room temperature to 600 ℃ for negative pressure degreasing; then vacuum sintering is carried out, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 5 ℃/min, and the time lasts for 60 min; finally, continuously introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa, heating from 900 ℃ to 1200 ℃ at the speed of 3 ℃/min, and keeping the temperature for 180 min; cooling to obtain the product. According to the invention, oxalic acid is adopted to carry out degreasing on the titanium alloy injection blank, inert gas is used for protection in the degreasing and sintering processes, no oxidation and no recarburization are ensured in the degreasing process, and alloy powder in the titanium alloy is prevented from reacting with oxygen/carbon through discontinuous vacuum and partial pressure sintering, so that a high-performance titanium alloy workpiece is obtained after sintering is completed.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method of sintering a powder injection molded titanium alloy, the method comprising:
putting the titanium alloy injection blank into a degreasing furnace, adding oxalic acid into the degreasing furnace, introducing argon, and degreasing at the degreasing temperature of 140 ℃ to obtain a degreased part;
putting the degreased part into a high-vacuum metal furnace, introducing argon into the high-vacuum metal furnace, and heating the high-vacuum metal furnace from room temperature to 600 ℃ for negative pressure degreasing; then vacuum sintering is carried out, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 5 ℃/min, and the time lasts for 60 min; finally, continuously introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa, heating from 900 ℃ to 1200 ℃ at the speed of 3 ℃/min, and keeping the temperature for 180 min; cooling to obtain the product.
2. The method according to claim 1, wherein the specific method for performing negative pressure degreasing by introducing argon into the high vacuum metal furnace and raising the temperature from room temperature to 600 ℃ comprises the following steps:
introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, heating from room temperature to 250 ℃ at the heating rate of 2 ℃/min, and preserving heat for 120 min;
keeping the flow of argon unchanged, heating from 250 ℃ to 430 ℃ at a heating rate of 3 ℃/min, and keeping the temperature for 180 min;
keeping the flow of argon unchanged, heating from 430 ℃ to 600 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 240 min.
3. The method according to claim 1, wherein the specific method of cooling is as follows:
introducing argon into the high-vacuum metal furnace at the flow rate of 50L/min, keeping the pressure of the argon at 50KPa, cooling from 1200 ℃ to 600 ℃ at the speed of 3 ℃/min, and continuing air cooling until the temperature reaches the room temperature.
4. The method as claimed in claim 1, wherein the method for degreasing at the degreasing temperature of 140 ℃ by adding oxalic acid into a degreasing furnace and introducing argon comprises the following specific steps:
the degreasing temperature was set at 140 ℃ and oxalic acid was added to the furnace at a rate of 3g/min while keeping the temperature at 2m3Introducing argon into the degreasing furnace at the flow rate of/h, and continuously degreasing for 1 h; then keeping the degreasing temperature, continuously adding oxalic acid into the degreasing furnace at the speed of 5g/min, and adding oxalic acid into the furnace at the speed of 3m3Introducing argon into the degreasing furnace at the flow rate of/h, and degreasing for 3 h; and cooling to obtain a degreased part.
5. The method of claim 1, further comprising:
placing the titanium alloy injection blank into a degreasing furnace, and then pouring the titanium alloy injection blank into the degreasing furnace at a height of 2m3Filling argon into the degreasing furnace at a flow rate of/h, and flushing the degreasing furnace and the titanium alloy injection molded blank for 1 hour.
6. The method of claim 1, further comprising:
defatting for 3 hr, and adding 1m3And introducing argon into the degreasing furnace at a speed of/h for 1h, and cooling along with the furnace to obtain a degreased part.
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Application publication date: 20210903 |