CN107999756B - Method for preparing high-temperature alloy honeycomb heat insulation plate based on injection molding - Google Patents
Method for preparing high-temperature alloy honeycomb heat insulation plate based on injection molding Download PDFInfo
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- 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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Abstract
The invention relates to the technical field of metal injection molding, and particularly discloses a method for preparing a high-temperature alloy honeycomb heat-insulating plate based on injection molding. The method comprises the following steps: s1, preparing master alloy powder; s2, feeding and granulating; s3, injection molding; s4, degreasing; s5, sintering; s6, hot isostatic pressing; s7, solid solution, aging treatment and the like. The high-temperature alloy honeycomb heat-insulating plate prepared by the method can effectively avoid the defects of complex processing technology, high manufacturing cost and low size precision caused by the traditional brazing technology, and the comprehensive mechanical property of the prepared high-temperature alloy honeycomb heat-insulating plate is superior to that of a honeycomb plate prepared by the brazing method.
Description
Technical Field
The invention relates to the technical field of metal injection molding, in particular to a method for preparing a high-temperature alloy honeycomb heat-insulating plate based on injection molding.
Background
The excellent characteristics of the honeycomb plate enable the honeycomb plate to be widely applied to the fields of aerospace, trains, ships and buildings. The honeycomb panel is different in its constituent material because of the difference in the application field of the honeycomb panel. The requirements for the mechanical properties and the high-temperature properties of the cellular board applied to the aerospace field are undoubtedly stricter. The high-temperature alloy honeycomb plate is used as an outer panel of the aerospace vehicle thermal protection system, so that the internal structure of the aerospace vehicle can be prevented from overheating and overburning, and the aerospace vehicle thermal protection system can bear external large stress load.
The honeycomb core used by the existing common brazing method has the problems of component segregation, abnormal growth of crystal grains and the like, so that the toughness and the processing performance of the material are reduced, the excellent performance of the high-temperature alloy cannot be fully exerted, and in addition, the process of brazing the honeycomb plate has the defects of low processing precision, high post-processing cost and the like.
At present, the nickel-based high-temperature alloy powder for injection molding mainly adopts plasma rotating electrode atomization alloy powder or inert gas atomization alloy powder, the particle size of the high-temperature alloy powder prepared by plasma rotating electrode atomization is large, the proportion of fine powder (less than or equal to 10 mu m) suitable for an injection molding process is extremely low (less than or equal to 10%), the fine powder rate of the high-temperature alloy powder prepared by inert gas atomization is improved, but the fine powder rate is still low (less than or equal to 40%), so the material utilization rate is low, and the raw material cost is high. On the other hand, high temperature alloy powders have low sintering activity, often requiring long sintering times above 1280 ℃ and achieving relative densities above 96% after sufficient liquid phase formation. The high-temperature long-time sintering not only increases the energy and equipment consumption, but also makes the sintering deformation control more difficult due to the appearance of a large amount of liquid phase, the sintered product has larger deformation and low size percent of pass.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a high-temperature alloy honeycomb heat-insulating plate based on injection molding. The method has low production cost, and the prepared high-temperature alloy honeycomb thermal insulation board has high density and good mechanical property.
The technical problem to be solved by the invention is realized by the following technical scheme:
a method for preparing a high-temperature alloy honeycomb heat-insulating plate based on injection molding comprises the following steps:
s1, preparing master alloy powder: carrying out vacuum melting on the master alloy to obtain a master alloy ingot, and then crushing and screening the master alloy ingot to obtain master alloy powder;
s2, feeding and granulating: mixing master alloy powder and nickel carbonyl (Ni) powder to obtain mixed powder, adding a binder to carry out banburying, and crushing after banburying uniformly to obtain a feed material;
s3, injection molding: injecting the feed into a mould to obtain a honeycomb heat insulation board green body;
s4, degreasing: degreasing the green body, and removing the binder in the green body;
s5, sintering: transferring the degreased green body into a vacuum sintering furnace for sintering to obtain a sintered body;
s6, hot isostatic pressing: putting the sintered blank into a hot isostatic pressing furnace, and pressurizing at high temperature to obtain a fully-compact honeycomb plate;
s7, solid solution and aging treatment: heating the fully-compact honeycomb plate in a tubular sintering furnace to the gamma' -phase dissolution temperature, carrying out solution treatment, then carrying out water cooling, heating to the aging temperature, carrying out heat preservation, and carrying out furnace cooling to obtain the high-temperature alloy honeycomb heat-insulating plate.
Preferably, the master alloy in step S1 is formed by mixing two or more or all of the following elements: ni, Cr, Mo, Ti, Al, Co, B.
Further preferably, the master alloy in step S1 is formed by mixing the following elements in parts by weight:
still more preferably, the master alloy in step S1 is formed by mixing the following elements in parts by weight:
preferably, the vacuum melting in step S1 is to put the master alloy into a vacuum induction furnace for vacuum melting;
the vacuum melting process comprises the following steps: introducing argon at normal temperature for 30-60min, wherein the purity of argon is 99.999%, the flow of argon is 5L/min, and then vacuumizing to 10%-3Pa, heating to 1000 ℃ at the heating rate of 10 ℃/min, preserving heat for 10-20min, heating to 2000 ℃ at the heating rate of 10 ℃/min, preserving heat for 30-40min, heating to 2800 ℃ at the heating rate of 5 ℃/min, preserving heat for 30-40min, and air-cooling.
Preferably, the weight percentage of the master alloy powder in the mixed powder of step S2 is 30-60%.
Preferably, the mixed powder described in step S2 is added in an amount of 60-65% of the total volume of the mixed powder and the binder.
Preferably, the binder described in step S2 includes the following components in parts by weight:
preferably, the banburying in step S2 is performed in an internal mixer; the banburying process comprises the following steps: heating the pair roller temperature of the internal mixer to between 160 ℃ and 180 ℃, wherein the internal mixing time is 120min and 180min, and the rotating speed is 20-30 rpm.
Preferably, the specific method of injection molding described in step S3 is: the feed is put into an injection machine for heating, melting, pressurizing and injecting into a mould, and the mould cavity is cooled to obtain a honeycomb heat insulation board green body; wherein the mold temperature is 100-120 ℃, and the injection temperature is 180-190 ℃.
Preferably, the degreasing in step S4 is catalytic degreasing, and the specific method is as follows: putting the green body into a catalytic degreasing furnace, heating to 100-2Cleaning for 40-60min before, and introducing HNO3The retention time is 200-300min, and then N is introduced2Cleaning for 30-60min, wherein nitrogen flow is 2-5m3H, the acid introduction amount is 3-5 g/min.
Preferably, the sintering method in step S5 is specifically: the heating speed is 3 ℃/min, the heating temperature is 1150--3Pa。
Preferably, the hot isostatic pressing in step S6 is performed by: the heating speed is 5 ℃/min, the heating temperature is 1100-.
Preferably, the solution temperature of the gamma' phase in the step S7 is 1100-1200 ℃, and the solution treatment time is 1-2 h; the aging temperature is 750-.
Has the advantages that: (1) the high-temperature alloy honeycomb heat-insulating plate is prepared by a brand-new injection molding method, so that the defects of complex processing technology, high manufacturing cost and low size precision caused by the traditional brazing process can be effectively overcome, and the comprehensive mechanical property of the prepared high-temperature alloy honeycomb heat-insulating plate is superior to that of a honeycomb plate prepared by the brazing method; (2) in the invention, in the design of the components of the master alloy, the difficult-to-fuse gold elements (Cr, Mo, Ti, Al, Co and B) are prepared into the master alloy in advance, and are not added into the nickel-based alloy in the form of elemental substances, the driving potential of atom migration in the sintering process is improved by increasing the specific surface area and the lattice distortion of powder, so that the sintering temperature is reduced, the sintering process can be carried out under the condition that no liquid phase or only a small amount of liquid phase is generated, the sintering deformation caused by the liquid phase is effectively reduced, and the cost of raw material powder and the process energy consumption can be obviously reduced; (3) the nickel-based high-temperature alloy honeycomb heat-insulating plate prepared by the preparation method has the compactness of 99 percent, the plane compression strength of more than 13MPa, the bending strength of more than 180MPa, the tensile strength of more than 1200MPa, the yield strength of more than 950MPa, the microhardness of more than 380HV, the density and the mechanical property of the heat-insulating plate exceed those of a brazed honeycomb heat-insulating plate, and the heat-insulating plate has uniform crystal grains, no component segregation and excellent high-temperature mechanical property and corrosion resistance.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a high-temperature alloy honeycomb heat-insulating plate according to the invention.
FIG. 2 is a schematic view of a superalloy honeycomb insulating panel of the present invention.
FIG. 3 is a catalytic degreasing process curve of a preparation method of the high-temperature alloy honeycomb thermal insulation plate.
FIG. 4 is a sintering process curve of a method for making a superalloy honeycomb insulation panel.
FIG. 5 is a hot isostatic pressing process curve of a method of making a high temperature alloy honeycomb insulation panel.
FIG. 6 is a solution process curve of a method of making a superalloy honeycomb insulating panel.
FIG. 7 is an aging process curve of a method for making a superalloy honeycomb insulation panel.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way.
The product density test method in the embodiment of the invention is as follows: GB/T3850-2015 dense sintering metal material and a hard alloy density measuring method.
The bending strength test method of the product in the embodiment of the invention is as follows: GB/T228.1-2010 metallic Material tensile test first part room temperature test method.
The microhardness test method of the product in the embodiment of the invention is as follows: and (3) measuring the apparent hardness and microhardness of the GB/T9097-2016 sintered metal material (not including the hard alloy).
The method for testing the plane compression strength of the product in the embodiment of the invention is as follows: GJB130.5-86 glue joint aluminum honeycomb sandwich structure and core plane compression performance test method.
The bending strength test method of the product in the embodiment of the invention is as follows: a bending performance test method of a GJB130.9-86 bonded aluminum honeycomb sandwich structure.
Example 1: high-temperature alloy honeycomb heat-insulating plate prepared from mixed powder prepared by mixing master alloy powder and carbonyl nickel powder in ratio of 40:60
The preparation method of the high-temperature alloy honeycomb heat-insulating plate comprises the following steps:
s1, preparing master alloy powder: mixing 15 parts of Ni, 25 parts of Cr, 25 parts of Co, 14 parts of Al, 13 parts of Ti, 7.5 parts of Mo and 0.2 part of B to obtain a master alloy; smelting the master alloy in a vacuum smelting furnace to obtain a master alloy ingot, wherein the vacuum smelting process comprises the following steps: introducing argon at normal temperature for 40min, wherein the purity of argon is 99.999%, the flow of argon is 5L/min, and then vacuumizing to 10%-3Pa, heating to 1000 ℃ at a heating rate of 10 ℃/min, preserving heat for 10min, heating to 2000 ℃ at a heating rate of 10 ℃/min, preserving heat for 30min, heating to 2800 ℃ at a heating rate of 5 ℃/min, preserving heat for 30min, air-cooling, and mechanically crushing and vibrating and screening a mother alloy ingot to obtain mother alloy powder;
s2, feeding and granulating: mixing master alloy powder and carbonyl nickel powder according to the weight ratio of 40:60 to obtain mixed powder, placing the mixed powder and a binder in an internal mixer, heating to 160 ℃, wherein the rotating speed of the internal mixer is 20r/min, the internal mixing time is 120min, preparing a feed with the powder loading of 61 vol.%, and placing the feed in an impeller roller crusher to crush to obtain granular feed;
the binder consists of 88 parts of polyformaldehyde, 4 parts of polypropylene, 4 parts of high-density polyethylene, 2 parts of low-density polyethylene and 2 parts of stearic acid;
s3, injection molding: heating the granular feed in an injection machine to 180 ℃, cooling the granular feed in a die cavity to obtain a honeycomb heat insulation board green body, wherein the die temperature is 100 ℃;
s4, catalytic degreasing: putting the green body into a catalytic degreasing furnace, heating to 100 ℃ at the heating rate of 5 ℃/min, and introducing 2.5m of flow3The first flushing is carried out for 60min by nitrogen gas, and then HNO is introduced3Defatting for 240min, introducing acid at a speed of 3g/min, and introducing 3m3The nitrogen per hour is used for post-flushing for 60 min;
s5, sintering: sintering the degreased blank in vacuum atmosphere with the vacuum degree of 10-3Pa, sintering temperature of 1200 ℃, heat preservation time of 90min, heating element being molybdenum wire;
s6, hot isostatic pressing: putting the sintered blank into a hot isostatic pressing furnace, wherein the temperature is 1100 ℃, the pressure is 150MPa, and the heat preservation time is 60min to obtain a fully-compact honeycomb heat insulation plate;
s7, solid solution and aging treatment: the fully-compact honeycomb heat insulation board is subjected to solution treatment at 1150 ℃ for 2h, then is subjected to water cooling, and then is subjected to aging treatment at 780 ℃ for 12 h.
Through detection, the density of the honeycomb heat insulation board obtained by the method of the embodiment is 99%, the plane compression strength is 13.6MPa, the bending strength is 185MPa, the tensile strength is 1250MPa, the yield strength is 960MPa, and the microhardness is 360 HV.
Example 2: high-temperature alloy honeycomb heat-insulating plate prepared from mixed powder prepared by mixing master alloy powder and carbonyl nickel powder in proportion of 50:50
The preparation method of the high-temperature alloy honeycomb heat-insulating plate comprises the following steps:
s1, preparing master alloy powder: mixing 32 parts of Ni, 20 parts of Cr, 20 parts of Co, 11 parts of Al, 10 parts of Ti, 6 parts of Mo and 0.2 part of B to obtain a master alloy; smelting the master alloy in a vacuum smelting furnace to obtain a master alloy ingot, wherein the vacuum smelting process comprises the following steps: introducing argon at normal temperature for 30min, wherein the purity of the argon is 99.999 percent and the argon isThe flow rate is 5L/min, and then the vacuum is pumped to 10-3Pa, heating to 1000 ℃ at a heating rate of 10 ℃/min, preserving heat for 20min, heating to 2000 ℃ at a heating rate of 10 ℃/min, preserving heat for 40min, heating to 2800 ℃ at a heating rate of 5 ℃/min, preserving heat for 40min, air-cooling, and mechanically crushing and vibrating and screening a mother alloy ingot to obtain mother alloy powder;
s2, feeding and granulating: mixing the master alloy powder and the carbonyl nickel powder according to the weight ratio of 50:50 to obtain mixed powder, placing the mixed powder and a binder in an internal mixer, heating to 160 ℃, wherein the rotating speed of the internal mixer is 25r/min, the internal mixing time is 180min, preparing a feed with the powder loading capacity of 64 vol.%, and placing the feed in an impeller roller crusher for crushing to obtain granular feed;
the binder consists of 85 parts of polyformaldehyde, 4 parts of polypropylene, 5 parts of high-density polyethylene, 4 parts of low-density polyethylene and 2 parts of stearic acid;
s3, injection molding: heating the granular feed to 190 ℃ in an injection machine, cooling the granular feed in a mold cavity to obtain a honeycomb heat insulation board green body, wherein the mold temperature is 110 ℃;
s4, catalytic degreasing: putting the green body into a catalytic degreasing furnace, heating to 110 ℃ at the heating rate of 5 ℃/min, and introducing 3m of flow3The first flushing is carried out for 60min by nitrogen gas, and then HNO is introduced3Defatting for 300min, introducing acid at a speed of 3.5g/min, and introducing 3.5m3The nitrogen per hour is used for post-flushing for 60 min;
s5, sintering: sintering the degreased blank in vacuum atmosphere with the vacuum degree of 10-3Pa, the sintering temperature is 1250 ℃, the heat preservation time is 180min, and the heating element is a molybdenum wire;
s6, hot isostatic pressing: putting the sintered blank into a hot isostatic pressing furnace, wherein the temperature is 1150 ℃, the pressure is 200MPa, and the heat preservation time is 120min to obtain a fully-compact honeycomb heat insulation plate;
s7, solid solution and aging treatment: the fully-compact honeycomb heat insulation plate is subjected to solution treatment at 1200 ℃ for 1h, then is subjected to water cooling, and then is subjected to aging treatment at 850 ℃ for 36 h.
Through detection, the density of the honeycomb heat insulation board obtained by the method of the embodiment is 99%, the plane compression strength is 14.0MPa, the bending strength is 190MPa, the tensile strength is 1200MPa, the yield strength is 990MPa, and the microhardness is 370 HV.
Claims (5)
1. A method for preparing a high-temperature alloy honeycomb heat-insulating plate based on injection molding is characterized by comprising the following steps:
s1 preparation of master alloy powder: carrying out vacuum melting on the master alloy to obtain a master alloy ingot, and then crushing and screening the master alloy ingot to obtain master alloy powder;
s2, feeding and granulating: mixing the master alloy powder and the carbonyl nickel powder to obtain mixed powder, then adding a binder to carry out banburying, and crushing after the banburying is uniform to obtain a feed;
s3, injection molding: injecting the feed into a mould to obtain a honeycomb heat insulation board green body;
s4 degreasing: degreasing the green body, and removing the binder in the green body;
s5, sintering: transferring the degreased green body into a vacuum sintering furnace for sintering to obtain a sintered body;
s6, hot isostatic pressing: putting the sintered blank into a hot isostatic pressing furnace, and pressurizing at high temperature to obtain a fully-compact honeycomb plate;
s7, solid solution and aging treatment: heating the fully-compact honeycomb plate to a gamma' -phase dissolution temperature in a tubular sintering furnace, carrying out solution treatment, then carrying out water cooling, heating to an aging temperature, carrying out heat preservation, and carrying out furnace cooling to obtain a high-temperature alloy honeycomb heat insulation plate;
the master alloy in the step S1 is prepared by mixing the following elements in parts by weight:
15-32 parts of Ni;
20-25 parts of Cr;
20-25 parts of Co;
11-14 parts of Al;
10-13 parts of Ti;
6-7.5 parts of Mo;
0.1-0.2 part of B;
the vacuum melting in the step S1 is to put the master alloy into a vacuum induction furnace for vacuum melting;
the vacuum melting process comprises the following steps: introducing argon at normal temperature for 30-60min, wherein the purity of argon is 99.999%, the flow of argon is 5L/min, and then vacuumizing to 10%-3Pa, heating to 1000 ℃ at the heating rate of 10 ℃/min, preserving heat for 10-20min, heating to 2000 ℃ at the heating rate of 10 ℃/min, preserving heat for 30-40min, heating to 2800 ℃ at the heating rate of 5 ℃/min, preserving heat for 30-40min, and then air-cooling;
step S2, the weight percentage of master alloy powder in the mixed powder is 30-60%; the adding amount of the mixed powder in the step S2 is 60-65% of the total volume of the mixed powder and the binder;
the binder described in step S2 contains the following components in parts by weight:
80-90 parts of polyformaldehyde;
1-4 parts of polypropylene;
2-6 parts of high-density polyethylene;
2-6 parts of low-density polyethylene;
1-8 parts of stearic acid.
2. The method of claim 1, wherein the banburying of step S2 is in
The preparation is carried out in an internal mixer; the banburying process comprises the following steps: heating the pair roller of the internal mixer to the temperature of 160-180 ℃, wherein the internal mixing time is 120-180min, and the rotating speed is 20-30 rpm;
the specific injection molding method described in step S3 is: the feed is put into an injection machine for heating, melting, pressurizing and injecting into a mould, and the mould cavity is cooled to obtain a honeycomb heat insulation board green body; wherein the mold temperature is 100-120 ℃, and the injection temperature is 180-190 ℃.
3. The method according to claim 1, wherein the degreasing in step S4 is catalytic degreasing, and the method comprises: putting the green body into a catalytic degreasing furnace, and heatingIntroducing N at 100-2Cleaning for 40-60min before, and introducing HNO3The retention time is 200-300min, and then N is introduced2Cleaning for 30-60min, wherein nitrogen flow is 2-5m3H, the acid introduction amount is 3-5 g/min;
the specific sintering method in step S5 includes: the heating speed is 3 ℃/min, and the heating temperature is
1150-1250 ℃, the heat preservation time is 90-180min, the temperature reduction speed is 5 ℃/min, and the vacuum degree is 10-3Pa。
4. The method of claim 1, wherein the hot isostatic pressing in step S6 is performed by: the heating speed is 5 ℃/min, the heating temperature is 1100-.
5. The method as claimed in claim 1, wherein the γ' phase in step S7 has a dissolution temperature of 1100-1200 ℃ and a solution treatment time of 1-2 h; the aging temperature is 750-.
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| CN103240412A (en) * | 2013-05-22 | 2013-08-14 | 北京科技大学 | Method for preparing powder super-alloy by near net shape |
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| CN103639408A (en) * | 2013-12-10 | 2014-03-19 | 北京科技大学 | Method for preparing titanium aluminum intermetallic compound from hydrogenated titanium-aluminum alloy through short process |
| CN104451225A (en) * | 2014-11-23 | 2015-03-25 | 北京科技大学 | Preparation method of superalloy composite material with double interconnected structure |
| CN106756148A (en) * | 2016-12-05 | 2017-05-31 | 北京科技大学 | The method that a kind of foundry alloy method of low oxygen content prepares MIM418 alloys |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240412A (en) * | 2013-05-22 | 2013-08-14 | 北京科技大学 | Method for preparing powder super-alloy by near net shape |
| CN103295770A (en) * | 2013-06-25 | 2013-09-11 | 李超 | Method for preparing composite bonded permanent magnet |
| CN103639408A (en) * | 2013-12-10 | 2014-03-19 | 北京科技大学 | Method for preparing titanium aluminum intermetallic compound from hydrogenated titanium-aluminum alloy through short process |
| CN104451225A (en) * | 2014-11-23 | 2015-03-25 | 北京科技大学 | Preparation method of superalloy composite material with double interconnected structure |
| CN106756148A (en) * | 2016-12-05 | 2017-05-31 | 北京科技大学 | The method that a kind of foundry alloy method of low oxygen content prepares MIM418 alloys |
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