CN111451498A - Degreasing method for powder metallurgy sintering - Google Patents
Degreasing method for powder metallurgy sintering Download PDFInfo
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- CN111451498A CN111451498A CN202010131961.1A CN202010131961A CN111451498A CN 111451498 A CN111451498 A CN 111451498A CN 202010131961 A CN202010131961 A CN 202010131961A CN 111451498 A CN111451498 A CN 111451498A
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- 238000005245 sintering Methods 0.000 title claims abstract description 39
- 238000005238 degreasing Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 38
- 238000001816 cooling Methods 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 150000002632 lipids Chemical class 0.000 claims abstract description 28
- 239000011261 inert gas Substances 0.000 claims abstract description 22
- 238000009833 condensation Methods 0.000 claims abstract description 16
- 230000005494 condensation Effects 0.000 claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000000110 cooling liquid Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 239000004519 grease Substances 0.000 abstract description 5
- 230000003749 cleanliness Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000004321 preservation Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005057 refrigeration Methods 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a degreasing method for powder metallurgy sintering, which comprises the steps of filling a sintering blank into a heating zone of a vacuum sintering furnace, vacuumizing the furnace until the vacuum degree is lower than 1Pa, introducing inert gas while vacuumizing, keeping the air pressure in the furnace between 150 Pa and 200Pa, starting heating to heat the furnace to 200-800 ℃ to gasify lipid additives in the sintering blank, driving the gasified lipid to flow to a spiral condensation well by the inert gas, spirally advancing along a cooling spiral air passage, cooling to the temperature of lower than 100 ℃, and condensing and recovering the lipid. By the method, the grease condensed on the wall of the vacuum furnace is greatly reduced, the carbon content in the material is reduced, and the material performance is improved; the grease-containing gas makes grease and gas fully separate through the spiral condensation well, so that the cleanliness is improved, the vacuum equipment is protected, the maintenance frequency of the equipment is reduced, the service life of the equipment is prolonged, and the environmental pollution is reduced.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a degreasing method for powder metallurgy sintering.
Background
In most powder metallurgy materials, the carbon content has a great influence on the properties of the material, and is brought in by impurities of the material itself and additives, the most important of which are additives, which may be molding agents, lubricants, mold release agents, etc. In the manufacturing process, a section of process is specially used for degreasing materials in the vacuum sintering process of a vacuum sintering furnace, specifically, a vacuum pump group is used for vacuumizing the furnace, the temperature is raised according to a preset degreasing temperature curve, an additive is gradually gasified and is pumped out by a vacuum pump group along with the temperature rise in the furnace body, the stripped grease passes through a baffle cooling well, and gas is condensed into liquid when passing through the baffle and is condensed into a recovery tank.
The above method has the following problems: (1) because the air pressure is lower, a part of lipids are not discharged in time and are carbonized in a vacuum furnace, and the carbon content of the material is influenced by carbonization at high temperature; (2) in the existing cooling well structure, gas condensation is insufficient, and residual lipid can enter an exhaust pipeline and vacuum equipment, so that the lipid is accumulated in the pipeline and pollutes the vacuum equipment, and the use of the equipment is influenced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a degreasing method for powder metallurgy sintering with better comprehensive effect.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention provides a degreasing method for powder metallurgy sintering, which specifically comprises the following steps:
1) loading the sintering blank into a heating zone of a vacuum sintering furnace;
2) vacuumizing the vacuum sintering furnace by adopting a vacuum pump set;
3) in the degreasing stage, when the vacuum degree in the furnace is lower than 1Pa, introducing inert gas while vacuumizing to maintain the air pressure in the furnace between 150 Pa and 200Pa, starting heating to heat the furnace to 200-800 ℃ to gasify the lipid additives of the sintered blank, and leading the gasified lipid to flow to an air extraction pipeline connected with a vacuum pump set under the drive of the inert gas;
4) leading the fat-containing gas to enter a spiral condensation well; the spiral condensation well is communicated with the air extraction pipeline and is provided with a cooling spiral air passage, so that the fat-containing gas spirally advances along the cooling spiral air passage and is cooled to be less than 100 ℃, and the fat is condensed and then flows back to the recovery container.
Optionally, in the step 3), the temperature rise curve of the degreasing section is to rise to 200-800 ℃ at a speed of less than 50 ℃/min and keep the temperature for 30-240 min.
Optionally, in the step 3), the temperature rise curve of the degreasing section is to rise to 200-400 ℃ and keep the temperature for 30-90min, and then rise to 400-800 ℃ and keep the temperature for 30-90 min.
Optionally, the vacuum sintering furnace includes a vacuum chamber and a heat insulation cylinder located in the vacuum chamber, and the heat insulation cylinder forms the heating zone; and 3), enabling the inert gas to enter between the cavity wall of the vacuum cavity and the heat insulation cylinder until the gas pressure of the inert gas is higher than that of the heating area, and enabling the inert gas to enter the heating area under the action of pressure.
Optionally, the vacuum sintering furnace is provided with an air inlet channel for introducing the inert gas, and the air inlet channel and the air exhaust pipeline are located on two opposite sides of the heat insulation cylinder.
Optionally, the spiral condensation well includes a shell, a central column, a spiral sheet and a refrigeration device, the spiral sheet is fitted between the shell and the central column to form the cooling spiral air passage, and the refrigeration device is disposed on the spiral sheet; the casing be equipped with cooling spiral air flue both ends complex air inlet and gas outlet, the casing still is equipped with the liquid outlet, recovery vessel locates the liquid outlet below.
Optionally, the air inlet is located at the lower part of the housing, and the air outlet is located at the upper part of the housing; and 4), enabling the fat-containing gas to pass through the cooling spiral gas channel from bottom to top.
Optionally, the refrigeration device includes a cooling pipe, the cooling pipe is coiled on the spiral sheet, and a cooling liquid is introduced into the cooling pipe.
Optionally, the water inlet and the water outlet of the cooling pipe are arranged at the lower end of the shell, the cooling pipe comprises two sections extending along the spiral piece in a spiral manner, and the two sections are communicated with the top of the spiral piece.
Optionally, the lipid additive content of the sintered blank is 0.2 wt% to 6 wt%.
The invention has the beneficial effects that:
(1) the gasified lipid is driven by the inert gas to be discharged out of the vacuum furnace, the condensed lipid on the wall of the vacuum furnace is greatly reduced, the carbon content in the material is reduced, and the material performance is improved;
(2) the grease-containing gas is fully separated from the gas through the cooling spiral gas passage, so that the cleanliness is improved, the vacuum equipment is protected, the maintenance frequency of the equipment is reduced, the service life of the equipment is prolonged, and the environmental pollution is reduced.
Drawings
FIG. 1 is a schematic diagram of the degreasing method of the present invention;
FIG. 2 is a schematic view of a vacuum sintering furnace with arrows indicating the gas flow direction;
fig. 3 is a schematic diagram of a spiral condensate well, wherein arrows indicate gas flow directions.
Detailed Description
The degreasing method of the powder metallurgy sintering according to the present invention will be further explained with reference to the drawings and the specific examples.
The degreasing method is realized through the structure shown in the figure 1, and comprises a vacuum sintering furnace 1, an air extraction pipeline 2, a spiral condensation well 3 and a vacuum pump set 4, wherein the vacuum sintering furnace 1 is communicated with the vacuum pump set 4 through the air extraction pipeline 2 so as to realize that the vacuum pump set 4 carries out vacuum-pumping operation on the vacuum sintering furnace 1, and the spiral condensation well 3 is communicated with the air extraction pipeline 2.
Referring to fig. 2, the vacuum sintering furnace 1 includes a vacuum chamber 11 and a heat insulating cylinder in the vacuum chamber 11, the heat insulating cylinder including a heat insulating device 12 and a heating element 13 in the heat insulating device, a heating zone being formed in the heat insulating cylinder, and a sintered blank 5 being placed in the heating zone. The vacuum sintering furnace 1 is provided with an air inlet channel 14 for introducing inert gas, and the air inlet channel 14 and the air exhaust pipeline 2 are positioned at two opposite sides of the heat insulation cylinder. And (3) putting the sintering blank 5 into a heating area of a vacuum sintering furnace 1, and vacuumizing the vacuum sintering furnace by using a vacuum pump set 4. The sintered blank 5 contains lipid additives such as a binder, and the content of the lipid additives is 0.2-6 wt%.
In the degreasing stage, when the degree of vacuum in the furnace is less than 1Pa, the gas inlet channel 14 is opened and inert gas is introduced while vacuumizing, so that the pressure in the furnace is maintained between 150 Pa and 200Pa, and heating is started to heat the furnace to 200-800 ℃. Specifically, inert gas is introduced between the wall of the vacuum chamber 11 and the heat insulating cylinder 12 until the gas pressure is higher than that of the heating zone, and the inert gas enters the heating zone under the pressure and flows to the gas exhaust pipeline 2 through the gas exhaust action of the vacuum pump set 4. At the above-mentioned heating temperature, the lipid additive of the sintered blank 5 is gasified, and the gasified lipid is driven by the inert gas to flow into the gas exhaust pipeline 2. The temperature rise curve of the degreasing section is to rise to 200-800 ℃ at a speed of below 50 ℃/min and keep the temperature for 30-240 min, more preferably a sectional heating mode, a heat preservation section is arranged between 200 ℃ and 300 ℃ and is mainly used for removing some adsorbed gas and water vapor, and the heat preservation time is about 30-90 min; a heat preservation section is arranged between 300 ℃ and 550 ℃ and is mainly used for removing the lipid in the material, and the heat preservation time is about 30-90 min. And when the air pressure is increased to more than 1Pa in the heating or heating process, starting introducing inert gas to keep the air pressure at about 150-200 Pa until the heat preservation time is over. In the whole degreasing process, the pressure of the heating zone is maintained between 150 Pa and 200Pa by controlling the flow of the inert gas, so that the gasified lipid is fully discharged out of the vacuum sintering furnace 1. After being discharged from the vacuum sintering furnace 1, the fat-containing gas enters a spiral condensation well 3 through an air exhaust pipeline 2.
Referring to fig. 3, the spiral type condensation well 3 includes a shell 31, a central column 32, a spiral sheet 33, a refrigerating device 34 and a cold trap 35, the spiral sheet 33 is fitted between the shell 31 and the central column 32 to form a cooling spiral air passage, and the refrigerating device 34 is provided on the spiral sheet 33. The housing 31 is provided with an air inlet 311 and an air outlet 312 which are matched with two ends of the cooling spiral air passage, wherein the air inlet 311 is positioned at the lower part of the housing 31, and the air outlet 312 is positioned at the upper part of the housing 31. The refrigerating device 34 comprises a cooling pipe which is coiled on the spiral sheet 33 and is internally filled with cooling liquid; the water inlet 341 and the water outlet 342 of the cooling pipe are disposed at the lower end of the housing 31, and as an example of a structure, the cooling pipe includes two sections extending spirally along the spiral piece, and the two sections are communicated with the top of the spiral piece 33, so that the cooling effect of the spiral piece 33 is achieved. The housing 31 is further provided with a liquid outlet 313, and a recovery container is arranged below the liquid outlet 313. The fat-containing gas advances from bottom to top along the cooling spiral air passage and is uniformly and fully cooled, the lipid is condensed and flows downwards under the action of gravity, the condensed lipid flows back to a recovery container after being fully condensed by a cold trap 35, the temperature of the gas leaving the spiral condensation well 3 is less than 100 ℃, and the lipid and the gas are fully separated. The cleanliness of the gas leaving the spiral condensate well 3 is improved, avoiding the lipids entering the subsequent pipelines and vacuum equipment.
Example 1
By adopting the degreasing method, the neodymium iron boron sintered blank (35 SH (Nd 27.02 wt%, Dy 0.24 wt%, Ho 4.74 wt%, Fe 64.93 wt%, Co 1 wt%, Nb0.2 wt%, Cu0.15 wt%, Al 0.75wt%, Ga 0.2 wt%, B0.96 wt%) with the total rare earth content of 32 wt%) is placed into a heating zone of a vacuum sintering furnace, in the degreasing stage, when the furnace is vacuumized until the vacuum degree in the furnace is lower than 1Pa, argon is introduced while vacuumizing, the air pressure in the furnace is maintained at the air pressure in the following table, meanwhile, heating is started to raise the temperature in the furnace to 200 ℃ and keep the temperature for 60min, then the furnace is raised to 350 ℃ and kept the temperature for 60min, the fat-containing gas passes through a condensation well 3 and the temperature is reduced to be lower than 100 ℃, and the fat and the gas are fully separated spirally.
Comparative example 1
Except that the air pressure value is out of the range of this patent, the rest is the same as the example 1.
Comparative example 2
The same material as in example 1 was placed in a heating zone of a vacuum sintering furnace, and the atmosphere pressure was maintained at about 0.2Pa before degreasing by non-gas-permeable evacuation, and the temperature was raised according to the temperature rise curve of example 1, and the atmosphere pressure increased with the temperature rise to about 20MPa, and after degreasing, the atmosphere pressure was maintained at about 0.2Pa by evacuation, and the lipid-containing gas was passed through a "" baffle cooling well.
Comparative example 2 the other processes and parameters were the same as in example 1, and no mention of processes and parameters was made that are generally set up in the art.
The results of the product performance tests obtained in example 1 and comparative example are given in the following table:
under the same formula, compared with a comparative example, the remanence of the preferred embodiment of the application is improved by 0.2-1.0 kGs, the carbon content is reduced from more than 1200ppm to about 600ppm, and the performance of the material is improved.
Example 2
Referring to the degreasing method of example 1, neodymium iron boron sintered blanks (35 SH (Nd 27.02 wt%, Dy 0.24 wt%, Ho 4.74 wt%, Fe 64.93 wt%, Co 1 wt%, nb0.2wt%, cu 0.15wt%, Al0.75 wt%, Ga 0.2 wt%, B0.96 wt%) with different lipid additive contents were placed in a heating zone of a vacuum sintering furnace, and in a degreasing stage, when the furnace was evacuated to a degree of vacuum of less than 1Pa, argon was introduced while evacuating, so that the pressure in the furnace was maintained at 180Pa, and at the same time heating was started to raise the temperature of the gas in the furnace to 200 ℃ and keep the temperature for 60min, and then to 350 ℃ and keep the temperature for 60min, and the lipid-containing gas was passed through a spiral condensation well and the temperature was lowered to less than 100 ℃, and the lipids and the gas were sufficiently separated.
Comparative example 3
Reference is made to comparative example 2.
The results of the product performance tests obtained are given in the following table:
the above examples are only intended to further illustrate the degreasing method of powder metallurgy sintering of the present invention, but the present invention is not limited to the examples, and any simple modification, equivalent change and modification made to the above examples according to the technical spirit of the present invention fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. A degreasing method for powder metallurgy sintering is characterized by comprising the following steps:
1) loading the sintering blank into a heating zone of a vacuum sintering furnace;
2) vacuumizing the vacuum sintering furnace by adopting a vacuum pump set;
3) in the degreasing stage, when the vacuum degree in the furnace is lower than 1Pa, introducing inert gas while vacuumizing to maintain the air pressure in the furnace between 150 Pa and 200Pa, starting heating to heat the furnace to 200-800 ℃ to gasify the lipid additives of the sintered blank, and leading the gasified lipid to flow to an air extraction pipeline connected with a vacuum pump set under the drive of the inert gas;
4) leading the fat-containing gas to enter a spiral condensation well; the spiral condensation well is communicated with the air extraction pipeline and is provided with a cooling spiral air passage, so that the fat-containing gas spirally advances along the cooling spiral air passage and is cooled to be less than 100 ℃, and the fat is condensed and then flows back to the recovery container.
2. Degreasing method according to claim 1, characterized in that: in the step 3), the temperature rise curve of the degreasing section is to rise to 200-800 ℃ at a speed of below 50 ℃/min and keep the temperature for 30-240 min.
3. Degreasing method according to claim 2, characterized in that: in the step 3), the temperature rise curve of the degreasing section is that the temperature rises to 200-300 ℃ and is kept for 30-90min, and then the temperature rises to 300-800 ℃ and is kept for 30-90 min.
4. Degreasing method according to claim 1, characterized in that: the vacuum sintering furnace comprises a vacuum cavity and a heat insulation cylinder positioned in the vacuum cavity, and the heating area is formed in the heat insulation cylinder; and 3), enabling the inert gas to enter between the cavity wall of the vacuum cavity and the heat insulation cylinder until the gas pressure of the inert gas is higher than that of the heating area, and enabling the inert gas to enter the heating area under the action of pressure.
5. Degreasing method according to claim 4, characterized in that: the vacuum sintering furnace is provided with an air inlet channel for introducing the inert gas, and the air inlet channel and the air exhaust pipeline are positioned on two opposite sides of the heat insulation cylinder.
6. Degreasing method according to claim 1, characterized in that: the spiral condensation well comprises a shell, a central column, a spiral sheet and a refrigerating device, wherein the spiral sheet is matched between the shell and the central column to form the cooling spiral air passage, and the refrigerating device is arranged on the spiral sheet; the casing be equipped with cooling spiral air flue both ends complex air inlet and gas outlet, the casing still is equipped with the liquid outlet, recovery vessel locates the liquid outlet below.
7. Degreasing method according to claim 6, characterized in that: the air inlet is positioned at the lower part of the shell, and the air outlet is positioned at the upper part of the shell; and 4), enabling the fat-containing gas to pass through the cooling spiral gas channel from bottom to top.
8. Degreasing method according to claim 6, characterized in that: the refrigerating device comprises a cooling pipe, the cooling pipe is spirally wound on the spiral sheet, and cooling liquid is filled in the cooling pipe.
9. Degreasing method according to claim 8, characterized in that: the water inlet and the water outlet of the cooling pipe are arranged at the lower end of the shell, the cooling pipe comprises two sections which extend along the spiral of the spiral piece, and the two sections are communicated with the top of the spiral piece.
10. Degreasing method according to claim 1, characterized in that: the lipid additive content of the sintering blank is 0.2-6 wt%.
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Cited By (3)
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| CN113218188A (en) * | 2021-04-14 | 2021-08-06 | 蓝山县金山川粉末冶金有限公司 | Oil discharge device for powder metallurgy processing |
| CN114309608A (en) * | 2021-12-29 | 2022-04-12 | 西南大学 | Tube furnace and method for releasing green compact forming agent from tube furnace |
| CN114589306A (en) * | 2021-11-20 | 2022-06-07 | 蓝山县金山川粉末冶金有限公司 | Powder metallurgy degreasing and oil discharging system |
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