CN111390178A - Metal injection molding stainless steel high-polishing material and preparation method and application thereof - Google Patents
Metal injection molding stainless steel high-polishing material and preparation method and application thereof Download PDFInfo
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- CN111390178A CN111390178A CN202010377420.7A CN202010377420A CN111390178A CN 111390178 A CN111390178 A CN 111390178A CN 202010377420 A CN202010377420 A CN 202010377420A CN 111390178 A CN111390178 A CN 111390178A
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
- B22F3/101—Changing atmosphere
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Abstract
The invention belongs to the technical field of new materials, and particularly discloses a stainless steel high-polishing material formed by metal injection and a preparation method and application thereof. The method comprises the following specific steps: uniformly mixing metal powder, boron (B) powder and a bonding agent; then forming a green body by metal injection; sintering the materials in nitrogen, vacuum and argon environments in sequence after catalytic degreasing, and then cooling the materials to obtain the high-polishing material. The invention realizes the surface layer sintering densification of the injection molding part by adjusting the sintering process and controlling the sintering atmosphere, and the part with rough surface is thrown out to expose the sintering dense layer in the polishing process, so the polished plane is a mirror surface. Meanwhile, a small amount of B element is added, so that a low-melting-point liquid phase is locally formed among the particles, particle rearrangement is promoted, pores among the particles are eliminated, and the wettability among the particles is realized to achieve surface layer sintering densification. Promotes the reduction of carbon and oxygen to form a compact layer on the surface of the sintered part so as to improve the polishing performance of the metal injection molding product.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a stainless steel high-polishing material formed by metal injection molding, and a preparation method and application thereof.
Background
Metal Injection Molding (MIM) is a new powder metallurgy near-net-shape forming technology which is introduced from the plastic Injection Molding industry, firstly, Metal powder and a binder meeting the MIM requirement are selected, then the powder and the binder are mixed into uniform feed material by adopting a proper method at a certain temperature, after granulation, Injection Molding is carried out, and the obtained formed blank is degreased and sintered and densified to form a final finished product. The manufacturing technology is suitable for mass production of fine metal parts with complex structures and is known as one of international 'hottest metal part forming technologies'. As shown in the figure, because the sintering is carried out by the powder particles, the metallurgical bonding is formed between the contact surfaces of the powder particles through diffusion along with the rise of the temperature in the sintering process to form a sintering neck, the sintering neck grows continuously along with the rise of the temperature, and finally, the sintering neck is spheroidized to form pores. So that generally 1-2% of pores remain in the interior after the metal injection molding material is sintered. When a metal injection molding material is used for polishing, the surface is generally required to be removed by 50-60 microns, internal pores are exposed, diffuse reflection is caused, the polished surface is frosted, and the polishing effect is poor. Therefore, since the same material has pores inside the injection-molded article, only the polishing performance is inferior to that of the plate material, and therefore, in many cases where mirror polishing is required, the application of the metal injection-molded part is limited due to the poor polishing performance.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a method for preparing a stainless steel high-polishing material by metal injection molding.
The invention also aims to provide the metal injection molding stainless steel high-polishing material prepared by the method.
The invention further aims to provide application of the obtained metal injection molding stainless steel high-polishing material in complex high-light parts.
The purpose of the invention is realized by the following scheme:
a preparation method of a metal injection molding stainless steel high polishing material comprises the following specific steps:
uniformly mixing metal powder, boron (B) powder and a binder; then forming a green body by metal injection; sintering the materials in nitrogen, vacuum and argon environments in sequence after catalytic degreasing, and then cooling the materials to obtain the high-polishing material.
The metal powder is at least one of 316L stainless steel metal powder, 304L stainless steel and 17-4PH stainless steel;
the adhesive is at least one of polyformaldehyde, polypropylene, stearic acid and polyethylene;
the mass ratio of the metal powder to the adhesive is 9: 1-4: 1.
The temperature for mixing is 160-210 ℃, and more preferably 190 ℃.
The using amount of the B powder meets the requirement that the mass percent of B in the obtained high-polishing material is 0.1-2%; preferably 0.5% to 1%.
The green body is sintered in nitrogen, vacuum and argon environments in sequence after catalytic degreasing, and then the cooling process is divided into fourteen stages: wherein the first to sixth stages are nitrogen thermal degreasing stages; the seventh section to the ninth section are vacuum internal combustion stages; the tenth to the tenth stages are argon partial pressure sintering stages; the thirteenth to fourteenth stages are cooling stages.
Preferably, the nitrogen thermal degreasing stage is that the temperature is kept at 350-650 ℃ for 350-450min under the nitrogen atmosphere; the vacuum internal combustion stage is to carry out heat preservation for 250-350 min at 650-1150 ℃ under vacuum; the argon partial pressure sintering stage is to preserve heat for 250-300 min at 1000-1400 ℃ in an argon atmosphere; and in the cooling stage, the temperature is reduced to 40-80 ℃ within 250-300 min under the argon atmosphere.
More preferably, the nitrogen hot degreasing stage comprises the following processes of heating the temperature of the first stage from room temperature to 350 ℃ in 45min under the condition that the nitrogen flow rate is 20L/min, heating the temperature of the second stage from 350 ℃ to 360 ℃ in 15min under the condition that the nitrogen flow rate is 20L/min, heating the temperature of the third stage from 360 ℃ to 450 ℃ in 60min under the condition that the nitrogen flow rate is 20L/min, keeping the temperature of the fourth stage at 450 ℃ for 120min under the condition that the nitrogen flow rate is 20L/min, heating the temperature of the fifth stage from 450 ℃ to 520 ℃ in 120min under the condition that the nitrogen flow rate is 20L/min, and heating the temperature of the sixth stage from 520 ℃ to 650 ℃ in 90min under the condition that the nitrogen flow rate is 20L/;
the process of the vacuum internal combustion stage comprises the following steps: the seventh stage is heating from 650 ℃ to 1020 ℃ in vacuum for 120min, the eighth stage is heating to 1120 ℃ in vacuum for 60min, and the ninth stage is heat preservation for 120min at 1120 ℃ in vacuum;
the process of the argon partial pressure sintering stage comprises the following steps that in the tenth stage, the temperature is increased from 1120 ℃ to 1240 ℃ through 60min under the condition that the argon flow is 10L/min, in the tenth stage, the temperature is increased from 1240 ℃ to 1360 ℃ through 150min under the condition that the argon flow is 10L/min, and in the tenth stage, the temperature is maintained for 60min at 1360 ℃ under the condition that the argon flow is 10L/min;
the cooling stage comprises a thirteenth stage of cooling from 1360 deg.C to 1020 deg.C in 45min under argon flow of 10L/min, and a fourteenth stage of cooling from 1020 deg.C to 60 deg.C in 240min by nitrogen forced cooling.
A stainless steel high polishing material for metal injection molding is prepared by the method.
The metal injection molding stainless steel high polishing material is applied to complex high-light parts.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention realizes the surface layer sintering densification of the injection molding part by adjusting the sintering process and controlling the sintering atmosphere, and the part with rough surface is thrown out to expose the sintering dense layer in the polishing process, so the polished plane is a mirror surface. Meanwhile, a small amount of B element is added, so that a low-melting-point liquid phase is locally formed among the particles, particle rearrangement is promoted, pores among the particles are eliminated, and the wettability among the particles is realized to achieve surface layer sintering densification. Promotes the reduction of carbon and oxygen to form a compact layer on the surface of the sintered part so as to improve the polishing performance of the metal injection molding product.
Drawings
FIG. 1 is a schematic diagram of the liquid phase formed between particles in the present invention.
FIG. 2 is an SEM of a 316L sintered part obtained in example 1.
FIG. 3 is an SEM of a 316L sintered part obtained in example 2.
FIG. 4 is an SEM of a 316L sintered part obtained in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference.
Example 1 element B is 0.5%
Mixing 316L metal powder with polyformaldehyde, polystyrene and stearic acid binder according to a mass ratio of 9:1, simultaneously adding 0.5% by mass of B powder, uniformly mixing in an internal mixer at 190 ℃, then forming a green body through metal injection, performing catalytic degreasing in a catalytic degreasing furnace through concentrated nitric acid at 120 ℃, sintering according to a sintering process, wherein the first to sixth stages are nitrogen thermal degreasing stages, the seventh to ninth stages are a stage of heating from room temperature to 350 ℃ through 45min under the condition that the nitrogen flow is 20L/min, the second stage is a stage of heating from 350 ℃ to 360 ℃ through 15min under the condition that the nitrogen flow is 20L/min, the third stage is a stage of heating from 360 ℃ to 450 ℃ through 60min under the condition that the nitrogen flow is 20L/min, the fourth stage is a stage of heating from 450 ℃ through 450 ℃ under the condition that the argon flow is 20L/min, the fifth stage is a stage of heating from 120 ℃ to 520 ℃ through 120min under the condition that the argon flow is 20 352/26/min, the sixth stage is a stage of heating from 450 ℃ to 450 ℃ through 200 min, the fourth stage is a stage of cooling from 120 ℃ through 120min under the argon flow is 120 ℃, the fourth stage of cooling from 120 ℃ through 10 min under the ten stages, the temperature is a stage of heating from 120 ℃, the ninth to 10 ℃, the ninth stage of the ninth stage is a stage of heating from 120 ℃ through 10 ℃, the ninth and the ninth stage of heating from 120 ℃ through 10 ℃, the nitrogen flow is a stage of heating from 120 ℃, the ninth and the ninth stage of the nitrogen flow is a stage of heating from 120 ℃ through 10 ℃, and the ninth stage of the ninth and 10 ℃, and the ninth stage of heating from 120 ℃, and 10 ℃, and the ninth stage of heating from 120 ℃ through 10 ℃, and the ninth stage of heating, and the ninth stage of heating from 120 ℃ through the fifth stage of the ninth stage of heating.
As shown in fig. 2, this example produced a sintered part of metal injection molding 316L, with a dense layer thickness of about 97 microns, which produced good polishing results.
Example 2 element B is 0.8%
Mixing 316L metal powder with polyformaldehyde, polystyrene and stearic acid binder according to the mass ratio of 9:1, simultaneously adding 0.8% by mass of B powder, uniformly mixing in an internal mixer at 190 ℃, then forming a blank through metal injection, carrying out catalytic degreasing at 120 ℃ by concentrated nitric acid in a catalytic degreasing furnace, sintering according to a sintering process, wherein the first to sixth stages are a nitrogen thermal degreasing stage, the seventh to ninth stages are a stage in which the temperature is increased from room temperature to 350 ℃ through 45min under the condition that the nitrogen flow is 20L/min, the second stage is a stage in which the temperature is increased from 350 ℃ to 360 ℃ through 15min under the condition that the nitrogen flow is 20L/min, the third stage is a stage in which the nitrogen flow is 20L/min, the temperature is increased from 360 ℃ to 450 ℃ through 60min under the condition that the nitrogen flow is 20 5639/min, the fourth stage is a stage in which the nitrogen flow is 20L/45/min, the temperature is maintained at 120 ℃ through 120min under the condition that the nitrogen flow is 120min, the temperature is increased from 450 ℃ to 360/10 ℃ through 120min under the fourth stage in which the argon flow is 20 ℃, the temperature is 10/10 ℃ through 10 ℃ under the condition that the temperature is 20L/10 min, the fifth stage in which the temperature is 20L/10 ℃ under the temperature is 120 ℃ under the condition that the temperature is 120min, the temperature is 120 ℃ under the ninth stage in which the ninth stage in which the temperature is 120 ℃, the temperature is 120 ℃ under the ninth stage in which the temperature is maintained from 120 ℃ under the ninth stage, and the ninth stage in which the ninth stage, and the temperature is 120 ℃ under the ninth stage, and the ninth stage in the temperature is 120 ℃ under the temperature is maintained under the ninth stage, and the ninth stage in which the temperature is 120.
FIG. 3 is an SEM of a 316L sintered part obtained in example 2, showing that a dense layer having a thickness of about 106 microns provides a good polishing effect.
Example 3 element B is 1%
Mixing 316L metal powder with polyformaldehyde, polystyrene and stearic acid binder according to the mass ratio of 9:1, simultaneously adding 1% by mass of B powder, uniformly mixing in an internal mixer at 190 ℃, then forming a blank by metal injection, carrying out catalytic degreasing by concentrated nitric acid in a catalytic degreasing furnace at 120 ℃, sintering according to the following sintering process, wherein the first to sixth stages are a nitrogen thermal degreasing stage, the seventh to ninth stages are a stage of heating from room temperature to 350 ℃ by 45min under the condition that the nitrogen flow is 20L/min, the second stage is a stage of heating from 350 ℃ to 360 ℃ by 15min under the condition that the nitrogen flow is 20L/min, the third stage is a stage of heating from 360 ℃ to 450 ℃ by 60min under the condition that the argon flow is 20L/min, the fourth stage is a stage of heating from 450 ℃ to 450 ℃ by 20L/min under the condition that the nitrogen flow is 20 3527/min, the fifth stage is a stage of heating from 450 ℃ to 450 ℃ by 120min under the condition that the argon flow is 20 5634/7/min, the fourth stage of heating from 450 ℃ to 60min under the argon flow is 120 ℃ from 120min under the ninth stage of 10/10 ℃ by 90/10 ℃, the fifth stage of heating from 120 ℃ under the vacuum cooling from 120 ℃ by 120min under the ninth stage of 20L/10 ℃ from 120 ℃ to 10 ℃ under the ninth stage of heating from 120 ℃, the ninth stage of heating from 120 ℃ under the ninth and the ninth stage of heating from 120min, and the ninth stage of heating from 120 ℃ under the ninth stage of the ninth and the ninth stage of the nitrogen flow is 120 ℃ under the ninth stage of the ninth and the ninth stages, and the ninth stages.
FIG. 4 is an SEM of the resulting 316L sintered part, showing that a dense layer of 312 microns in thickness resulted in a good polishing effect.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a metal injection molding stainless steel high polishing material is characterized by comprising the following specific steps:
uniformly mixing metal powder, boron powder and an adhesive; then forming a green body by metal injection; sintering the materials in nitrogen, vacuum and argon environments in sequence after catalytic degreasing, and then cooling the materials to obtain the high-polishing material.
2. The method of claim 1, wherein: the dosage of the B powder meets the requirement that the mass percent of B in the obtained high polishing material is 0.1-2%.
3. The production method according to claim 1 or 2, characterized in that: the green body is sintered in nitrogen, vacuum and argon environments in sequence after catalytic degreasing, and then the cooling process is divided into fourteen stages: wherein the first to sixth stages are nitrogen thermal degreasing stages; the seventh section to the ninth section are vacuum internal combustion stages; the tenth to the tenth stages are argon partial pressure sintering stages; the thirteenth to fourteenth stages are cooling stages.
4. The production method according to claim 3, characterized in that: the nitrogen thermal degreasing stage is to preserve heat at 350-650 ℃ for 450min in a nitrogen atmosphere; the vacuum internal combustion stage is to carry out heat preservation for 250-350 min at 650-1150 ℃ under vacuum; the argon partial pressure sintering stage is to preserve heat for 250-300 min at 1000-1400 ℃ in an argon atmosphere; and in the cooling stage, the temperature is reduced to 40-80 ℃ within 250-300 min under the argon atmosphere.
5. The preparation method according to claim 3, wherein the nitrogen thermal degreasing stage comprises a first stage of heating from room temperature to 350 ℃ in 45min at a nitrogen flow rate of 20L/min, a second stage of heating from 350 ℃ to 360 ℃ in 15min at a nitrogen flow rate of 20L/min, a third stage of heating from 360 ℃ to 450 ℃ in 60min at a nitrogen flow rate of 20L/min, a fourth stage of heating from 450 ℃ to 120min at a nitrogen flow rate of 20L/min, a fifth stage of heating from 450 ℃ to 520 ℃ in 120min at a nitrogen flow rate of 20L/min, and a sixth stage of heating from 520 ℃ to 650 ℃ in 90min at a nitrogen flow rate of 20L/min;
the process of the vacuum internal combustion stage comprises the following steps: the seventh stage is heating from 650 ℃ to 1020 ℃ in vacuum for 120min, the eighth stage is heating to 1120 ℃ in vacuum for 60min, and the ninth stage is heat preservation for 120min at 1120 ℃ in vacuum;
the process of the argon partial pressure sintering stage comprises the following steps that in the tenth stage, the temperature is increased from 1120 ℃ to 1240 ℃ through 60min under the condition that the argon flow is 10L/min, in the tenth stage, the temperature is increased from 1240 ℃ to 1360 ℃ through 150min under the condition that the argon flow is 10L/min, and in the tenth stage, the temperature is maintained for 60min at 1360 ℃ under the condition that the argon flow is 10L/min;
the cooling stage comprises a thirteenth stage of cooling from 1360 deg.C to 1020 deg.C in 45min under argon flow of 10L/min, and a fourteenth stage of cooling from 1020 deg.C to 60 deg.C in 240min by nitrogen forced cooling.
6. The method of claim 1, wherein the metal powder is at least one of metal powder of 316L stainless steel, 304L stainless steel, and 17-4PH stainless steel;
the adhesive is at least one of polyformaldehyde, polypropylene, stearic acid and polyethylene.
7. The method of claim 1, wherein: the mass ratio of the metal powder to the adhesive is 9: 1-4: 1.
8. The method of claim 1, wherein: the temperature for mixing is 160-210 ℃.
9. A metal injection molding stainless steel high polishing material prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the metal injection molded stainless steel high-gloss material of claim 9 in complex high-gloss parts.
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| CN113664200A (en) * | 2021-07-28 | 2021-11-19 | 深圳市泛海统联精密制造股份有限公司 | Method for preparing mirror-polished product by metal powder injection molding process |
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