CN102248167A - Quick zero-defect degreasing method for large-size extrusion forming blank - Google Patents
Quick zero-defect degreasing method for large-size extrusion forming blank Download PDFInfo
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- CN102248167A CN102248167A CN2011101862736A CN201110186273A CN102248167A CN 102248167 A CN102248167 A CN 102248167A CN 2011101862736 A CN2011101862736 A CN 2011101862736A CN 201110186273 A CN201110186273 A CN 201110186273A CN 102248167 A CN102248167 A CN 102248167A
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Abstract
The invention discloses a quick zero-defect degreasing method for a large-size extrusion forming blank, comprising the following steps of: feeding a formed blank into a solvent degreasing tank and adding a degreasing solvent at the same time, wherein the ratio of a liquid to a solid is 7:1-15:1; degreasing under the condition of constant temperature of 30-60 DEG C for 6-12h; taking out the degreased blank and drying the greased blank at the constant temperature of 30-50 DEG C for 0.5-1h; replacing the degreasing solvent and drying; repeating 2-3 times until the mass loss of a binding agent reaches 60-75 percent; and feeding a solvent greasing blank in a high-temperature degreasing furnace and raising the temperature to 600-850 DEG C in the atmosphere of vacuum or negative pressure to obtain the zero-defect large-size degreasing blank. According to the quick zero-defect degreasing method disclosed by the invention, the defects of long degreasing time of the large-size forming blank, poor degreasing shape retention and more greasing defects are overcome; in addition, two adopted degreasing processes are simple, easy to control and are widely applied in actual production.
Description
Technical field
The invention belongs to powder metallurgical technology, relate to a kind of defatting technology of powder near-net-shape.
Background technology
Powder injection forming (PIM) and powder extrusion forming (PEM) are development in recent years two kinds of powder metallurgy near-net-shape new technologies rapidly, be suitable for the machine-shaping of materials such as various metals, alloy, ceramic powders, particularly be shaped and be difficult to shape the material of method preparation such as compound, pottery etc. between carbide alloy, copper, steel, tungsten, refractory metal with routine, can be with these two kinds of technology, provide new technical method to the research and development of new material and products thereof.
The basic craft course of PIM and PEM is:
Body of powder+binding agent → mixing → injection or extrusion molding → remove binding agent → sintering
Wherein, the design of binding agent and the technology that removes thereof are PIM and PEM technology key of success, especially binding agent removes, be that defatting technology is the committed step that the restriction parts develop to large scale, big thickness or extremely thin heavy in section change direction in the whole technical process, conference causes that the time-consuming length of degreasing process, defective are many, process is difficult to control as the powder extrusion forming product size, has restricted the development of PEM industry.And along with the development of society, the demand of powder metallurgy special-shaped product is constantly increased, simultaneously requirements at the higher level have been proposed for large scale parts and big thick.Therefore, it is most important to study and develop the defatting technology method that is fit to preparation large scale parts product.
Fan Jinglian etc. are at China YouSe Acta Metallurgica Sinica (2001,11 (4): 651～641) go up report: adopt the mixture of multicomponent small molecular organic solvent that large scale injection moulding sample base is carried out solvent degreasing, when being big stick-means of intimidation solvent degreasing 24～30h of 20mm for diameter, the degreasing amount is 50%～60%, all the other binding agents can adopt hot degreasing process to remove, and this degreasing method length consuming time, efficient are low.Baojun Zhu etc. are at Journal of Materials Processing Technology (2003,142:487-492) go up employing condensing steam degreasing new method several powder injection forming large dimension specimens are carried out degreasing, the degreasing sample comprises that the disk specimen finish is 20mm, thick 4.2mm; Rectangular specimen is of a size of 6mm * 6mm * 42mm, and spherical specimen finish is 9mm, and the pole specimen finish is 8mm, long 68mm.Adopt this degreasing method, degreasing efficient height, degreasing base intensity is big, but has the degreasing plant complexity, and solvent vapo(u)r has bigger pollution to surrounding environment, and to operator's problem such as healthy unfavorable.(2008,63:3802-3809) upward report adopts the siphon degreasing method to I.M.Somasundram etc., has realized that quickly and easily diameter is the degreasing of the cylinder sample of 16mm, long 40mm at Chemical Engineering Science.Yet this degreasing method exists green compact surface and siphon powder to bond mutually causes product surface to pollute, and the cost height, less employing in production application.Zhou Jicheng etc. Journal of Materials Processing Technology (2003,137:21-24) go up by the hot degreasing heating rate of control meticulously, realized that diameter reaches the degreasing of the carbide alloy extruding rod of 20mm.T.Jardiel etc. Ceramics International (2009,35:2329-2335) report trace integration to adopt solvent degreasing and hot degreasing process, made the big L/D ratio tubing of wall thickness less than 200 μ m.
Summary of the invention
Purpose of the present invention is intended to explore a kind of defatting technology new method of powder near-net-shape green compact, to realize the fast defat of shaping base, guarantees degreasing base zero defect simultaneously, particularly can realize large scale shaping base simply, zero defect degreasing easily and fast.
A kind of quick zero defect degreasing method of large scale extrusion molding base may further comprise the steps:
1) the shaping base is put into the solvent degreasing groove, add degreasing solvent simultaneously, liquid-solid volume ratio is 7: 1～15: 1, and degreasing 6～12h under 30～60 ℃ constant temperature takes out the degreasing base at 30～50 ℃ of following freeze-day with constant temperature 0.5～1h;
2) change degreasing solvent, in above-mentioned steps 1) degreasing under the same terms, freeze-day with constant temperature, degreasing time is 2～6h;
3) repeating step 2) 2-3 time, reach 60～75% until the binding agent weight loss;
4) the solvent degreasing base is placed the high temperature debinding furnace, in vacuum (10
-1～10
-3Pa) or negative pressure (under 200～400Pa), rise to 600～850 ℃ of insulations, obtain zero defect large scale degreasing base.
Described degreasing solvent comprises normal heptane, dichloroethylene, chloroform or cyclohexane.
Step 1) and 2) constant temperature in is the constant temperature under the water bath condition.
Described binding agent is the paraffinic base compound binding agent.(the paraffinic base compound binding agent is the binding agent that belongs to a class routine, the all available the inventive method of this class removes, this is because the present invention carries out substep to binding agent to remove, at first solvent degreasing removes main component paraffin in the binding agent, and the subsequent thermal degreasing is degraded to small portion of residual composition in the binding agent and removed)
In the step 4), injected the N of 5vol.% at the high temperature debinding furnace
2Or Ar.
Intensification is the speed intensification with 2-5 ℃/min in the step 4).
Temperature retention time is 30～90min in the step 4).
Degreasing method involved in the present invention can realize quickly and easily that (degreasing of diameter or thickness 〉=20mm) guarantees degreasing base zero defect to large scale shaping base simultaneously.
The advantage and the good effect of invention
Powder near-net-shape defatting technology of the present invention has improved the shortcoming that large scale shaping base degreasing time is long, the degreasing conformality is poor, the degreasing defective is many.Degreasing process is simple and be easy to control, increases drying steps in the solvent degreasing process, makes that residual stress obtains discharging in the degreasing base, avoided the degreasing generation of defects, carry out 2-3 time circulating solvent degreasing simultaneously, can make the degreasing amount, improved degreasing efficient up to more than 70%.In the subsequent thermal skimming processes, adopt vacuum or negative pressure atmosphere, improved the conformality of degreasing base.Comprehensive solvent degreasing and the hot degreasing process of adopting, degreasing efficient height can be realized the zero defect degreasing of large scale shaping base quickly and easily.
Description of drawings
Fig. 1 is embodiment 1 a sample photo
Excellent base photo (Φ 24mm) before (a) degreasing wherein; (b) excellent base photo (Φ 24mm) after the degreasing; (c) excellent base fracture SEM photo before the degreasing; (d) excellent base fracture SEM photo after the degreasing
Fig. 2 is embodiment 2 sample photos
Excellent base photo (Φ 38mm) before (a) degreasing wherein; (b) excellent base photo (Φ 38mm) after the degreasing; (c) excellent base fracture SEM photo before the degreasing; (d) excellent base fracture SEM photo after the degreasing.
The specific embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1:
1. adopt the powder plasticizing extrusion forming technology, be prepared into the big L/D ratio tungsten-bast alloy rod base of Φ 24mm, used binding agent is the paraffinic base compound binding agent.
2. will push excellent base and put into the solvent degreasing groove, and add a certain amount of normal heptane simultaneously, liquid-solid ratio is 8: 1 (volume ratio).
2. adopt water bath with thermostatic control to regulate and control the degreasing solvent temperature, degreasing 8h under 40 ℃ condition.
3. the degreasing base is taken out and place thermostatic drying chamber, be incubated 0.5h down at 35 ℃.
4. the replacing degreasing solvent immerses the degreasing base in the normal heptane again, and skimming temp is 40 ℃, and degreasing time is 4h.
5. again the degreasing base is taken out and place thermostatic drying chamber dry, so repeatedly, soak solvent degreasing through 2 times, drying, the binding agent weight loss can reach 70%.
6. the solvent degreasing base is placed the high temperature debinding furnace, under vacuum atmosphere, rise to 650 ℃ and be incubated 1 hour and carry out the subsequent thermal degreasing, obtain the degreasing rod base of zero defect big L/D ratio Φ 24mm with 5 ℃/min programming rate.
7. with defatting technology method of the present invention, improved and pushed excellent base very easily produces defectives such as cracking in the solvent degreasing process deficiency, realized that big L/D ratio pushes the quick zero defect degreasing of excellent base.
Embodiment 2:
1. adopt the powder plasticizing extrusion forming technology, be prepared into the big L/D ratio tungsten-bast alloy rod base of Φ 38mm, used binding agent is the paraffinic base compound binding agent.
2. will push excellent base and put into the solvent degreasing groove, and add a certain amount of normal heptane simultaneously, liquid-solid ratio is 12: 1 (volume ratio).
2. adopt water bath with thermostatic control to regulate and control the degreasing solvent temperature, degreasing 10h under 45 ℃ condition.
3. the degreasing base is taken out and place thermostatic drying chamber, be incubated 1h down at 40 ℃.
4. the replacing degreasing solvent immerses the degreasing base in the normal heptane again, and skimming temp is 45 ℃, and degreasing time is 6h.
5. again the degreasing base is taken out and place thermostatic drying chamber dry, soak solvent degreasing through 2 times, drying, the binding agent weight loss is 62%.
6. the solvent degreasing base is placed the high temperature debinding furnace, under vacuum atmosphere, rise to 800 ℃ and be incubated 1 hour and carry out the subsequent thermal degreasing, obtain the degreasing rod base of zero defect big L/D ratio Φ 38mm with 3 ℃/min programming rate.
7. with defatting technology method of the present invention, realized that quickly and easily big thickness pushes the degreasing of excellent base, the degreasing rod base zero defect that obtains simultaneously.
Embodiment 3:
Traditional degreasing method and degreasing method of the present invention are used in contrast.
Traditional degreasing method is: hot degreasing or easy solvent degreasing+hot two step of degreasing degreasing process.
The powder plasticizing extrusion forming technology is adopted in experiment, is prepared into the big L/D ratio tungsten-bast alloy rod base of Φ 24mm, and used binding agent is the paraffinic base compound binding agent.Adopt traditional hot degreasing, traditional simple and easy hot degreasing+hot degreasing two step process and degreasing method of the present invention (being designated as M, N, F respectively) simultaneously, experimental result such as table 1.
The experimental result of the different degreasing methods of table 1 Φ 24mm rod base
Claims (7)
1. the quick zero defect degreasing method of a large scale extrusion molding base is characterized in that: may further comprise the steps:
1) the shaping base is put into the solvent degreasing groove, add degreasing solvent simultaneously, liquid-solid volume ratio is 7: 1～15: 1, and degreasing 6～12h under 30～60 ℃ constant temperature takes out the degreasing base at 30～50 ℃ of following freeze-day with constant temperature 0.5～1h;
2) change degreasing solvent, in above-mentioned steps 1) degreasing under the same terms, freeze-day with constant temperature, degreasing time is 2～6h;
3) repeating step 2) 2-3 time, reach 60～75% until the binding agent weight loss;
4) the solvent degreasing base is placed the high temperature debinding furnace, in vacuum 10
-1～10
-3Under Pa or the negative pressure 200～400Pa, rise to 600～850 ℃ of insulations, obtain zero defect large scale degreasing base.
2. method according to claim 1 is characterized in that described degreasing solvent comprises normal heptane, dichloroethylene, chloroform or cyclohexane.
3. method according to claim 1 is characterized in that, step 1) and 2) in constant temperature be constant temperature under the water bath condition.
4. method according to claim 1 is characterized in that, described binding agent is the paraffinic base compound binding agent.
5. method according to claim 1 is characterized in that, in the step 4), has injected the N of 5vol.% at the high temperature debinding furnace
2Or Ar.
6. method according to claim 1 is characterized in that, intensification is the speed intensification with 2-5 ℃/min in the step 4).
7. method according to claim 1 is characterized in that, temperature retention time is 30～90min in the step 4).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198449A (en) * | 2015-09-16 | 2015-12-30 | 广东工业大学 | Method for preparing photocuring-formed high-density ceramic |
| CN105330268A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Manufacturing method of laminated ceramics |
| CN105330266A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Preparation method of tooth-like special-shaped ceramics |
| CN107127337A (en) * | 2017-06-23 | 2017-09-05 | 昆山卡德姆新材料科技有限公司 | A kind of two-part degreasing method of powder injection molding shaping |
| CN113307633A (en) * | 2021-07-07 | 2021-08-27 | 杭州陶飞仑新材料有限公司 | Preparation method of rapidly sintered porous ceramic |
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| EP0160855B1 (en) * | 1984-04-12 | 1990-07-25 | Mitsubishi Corporation | A method for the freeze-pressure molding of metallic powders |
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| US20040057861A1 (en) * | 2002-09-25 | 2004-03-25 | University Of Rochester | Method and apparatus for the manufacture of high temperature materials by combustion synthesis and semi-solid forming |
| CN1974080A (en) * | 2006-12-15 | 2007-06-06 | 湖南大学 | Gradient negative pressure hot defatting technology for powder injecting formation |
| CN101293280A (en) * | 2008-06-16 | 2008-10-29 | 中南大学 | Method for producing molybdenum alloy gas vane with powder injection forming |
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2011
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| EP0160855B1 (en) * | 1984-04-12 | 1990-07-25 | Mitsubishi Corporation | A method for the freeze-pressure molding of metallic powders |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198449A (en) * | 2015-09-16 | 2015-12-30 | 广东工业大学 | Method for preparing photocuring-formed high-density ceramic |
| CN105330268A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Manufacturing method of laminated ceramics |
| CN105330266A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Preparation method of tooth-like special-shaped ceramics |
| CN107127337A (en) * | 2017-06-23 | 2017-09-05 | 昆山卡德姆新材料科技有限公司 | A kind of two-part degreasing method of powder injection molding shaping |
| CN113307633A (en) * | 2021-07-07 | 2021-08-27 | 杭州陶飞仑新材料有限公司 | Preparation method of rapidly sintered porous ceramic |
| CN113307633B (en) * | 2021-07-07 | 2022-11-22 | 杭州陶飞仑新材料有限公司 | Preparation method of rapidly sintered porous ceramic |
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Application publication date: 20111123 |