CN112517911A - High-nitrogen nickel-free stainless steel sintering process - Google Patents
High-nitrogen nickel-free stainless steel sintering process Download PDFInfo
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- CN112517911A CN112517911A CN202011420613.2A CN202011420613A CN112517911A CN 112517911 A CN112517911 A CN 112517911A CN 202011420613 A CN202011420613 A CN 202011420613A CN 112517911 A CN112517911 A CN 112517911A
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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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- 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
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Abstract
The invention discloses a high-nitrogen nickel-free stainless steel sintering process, which comprises the following steps: step one, preparing a high-nitrogen nickel-free stainless steel feed: mixing high-nitrogen nickel-free stainless steel powder and a binder according to a ratio of 8:1, uniformly mixing, and putting the obtained mixture into a feeding crusher to prepare granular feed with uniform size; step two, injection molding; step three, degreasing; step four, sintering and nitriding; step five, reducing and sintering argon; step six, secondary sintering and nitriding; and seventhly, carrying out solution treatment on the product to remove chromium nitride precipitates in the product. According to the invention, after the sintering defective product is subjected to Ar reduction, secondary sintering nitridation is carried out, and the sintering is qualified, so that the rejection rate is greatly reduced, the cost is reduced, and large-scale production can be realized.
Description
Technical Field
The invention relates to the technical field of stainless steel, in particular to a high-nitrogen nickel-free stainless steel sintering process.
Background
Austenitic stainless steel is one of the most important engineering materials, such as 316L, AISI and the like, due to the advantages of strong corrosion resistance, high ductility, no magnetism and the like, and is widely applied to industry. Nickel is one of elements that stabilize the austenite structure, and thus, conventional stainless steels contain a large amount of nickel. The nickel element has the problems of poor biocompatibility, high cost and the like, so that the application of the nickel element in the fields of consumer electronics and biomedicine is limited. In recent years, nitrogen has been introduced into austenitic stainless steel instead of nickel, and high-nitrogen nickel-free stainless steel has emerged. The solid solubility of nitrogen in austenite is much higher than that in liquid iron, and therefore, powder metallurgy for producing high nitrogen nickel-free stainless steel has irreplaceable advantages.
The powder injection molding-sintering nitriding process is an emerging process for producing high nitrogen nickel-free stainless steel and has already begun to be applied in industry. Although the high-nitrogen nickel-free stainless steel has many advantages compared with the traditional austenitic stainless steel, such as good biocompatibility, good corrosion resistance, higher strength and hardness, better stable austenitic structure and the like. However, the existing high-nitrogen stainless steel sintering process has industrial difficulties, and the main reasons are that the sintering is unstable, the sintering size fluctuation is large, and the mass production is not realized.
Disclosure of Invention
The invention aims to provide a high-nitrogen nickel-free stainless steel sintering process aiming at the defects of the prior art, the sintering defective product is subjected to Ar reduction and then subjected to secondary sintering nitridation, and the high-nitrogen nickel-free stainless steel is sintered to be qualified, so that the rejection rate is greatly reduced, the cost is reduced, and the large-scale production can be realized.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A high-nitrogen nickel-free stainless steel sintering process comprises the following steps:
step one, preparing a high-nitrogen nickel-free stainless steel feed: mixing high-nitrogen nickel-free stainless steel powder and a binder according to a ratio of 8:1, uniformly mixing, and putting the obtained mixture into a feeding crusher to prepare granular feed with uniform size;
step two, injection molding: molding the feed obtained in the step one in an injection molding machine to obtain an injection blank with an expected structure;
step three, degreasing: placing the injection blank obtained in the step two on a special ceramic jig, and degreasing the injection blank by using a special degreasing furnace to obtain a degreased part;
step four, sintering and nitriding: and (3) putting the degreased part prepared in the step three into a sintering furnace for nitriding and sintering to prepare the high-nitrogen nickel-free stainless steel sintered part, which comprises the following specific steps:
a. negative pressure degreasing: introducing nitrogen, and heating the furnace to 850 ℃;
b. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 850 ℃, and keeping the temperature for 60 min;
c. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising furnace temperature to 1050 ℃, and keeping the temperature for 60 min;
d. and (2) partial pressure sintering: introducing nitrogen, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then reducing the temperature of the furnace to 900 ℃;
e. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
step five, reduction and sintering by argon gas: and (3) placing the defective sintered part in the fourth step into the sintering furnace in the fourth step for argon reduction sintering to obtain a compact sintered part, which comprises the following specific steps:
f. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min;
g. partial pressure sintering: introducing argon, increasing partial pressure sintering pressure, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then reducing the furnace temperature to 1050 ℃;
h. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
step six, secondary sintering and nitriding: and (4) placing the compact sintered part prepared in the fifth step into the sintering furnace of the fourth step for secondary nitriding sintering to prepare a high-nitrogen nickel-free stainless steel product with stable size, and the specific steps are as follows:
i. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min;
j. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising furnace temperature to 1200 ℃, and keeping the temperature for 60 min; then reducing the furnace temperature to 1050 ℃;
k. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
and seventhly, carrying out solution treatment on the product to remove chromium nitride precipitates in the product.
Wherein the nitrogen content of the high-nitrogen nickel-free stainless steel feed in the first step is less than 0.3 percent.
And C, wherein the nitrogen content of the dense sintered part obtained in the fifth step is less than 0.5%.
Wherein the nitrogen content of the six-dimensionally stable high-nitrogen nickel-free stainless steel product of step six is greater than 0.65%.
The invention has the beneficial effects that: the invention relates to a high-nitrogen nickel-free stainless steel sintering process, which comprises the following steps of: step one, preparing a high-nitrogen nickel-free stainless steel feed: mixing high-nitrogen nickel-free stainless steel powder and a binder according to a ratio of 8:1, uniformly mixing, and putting the obtained mixture into a feeding crusher to prepare granular feed with uniform size; step two, injection molding: molding the feed obtained in the step one in an injection molding machine to obtain an injection blank with an expected structure; step three, degreasing: placing the injection blank obtained in the step two on a special ceramic jig, and degreasing the injection blank by using a special degreasing furnace to obtain a degreased part; step four, sintering and nitriding: and (3) putting the degreased part prepared in the step three into a sintering furnace for nitriding and sintering to prepare the high-nitrogen nickel-free stainless steel sintered part, which comprises the following specific steps: a. negative pressure degreasing: introducing nitrogen, and heating the furnace to 850 ℃; b. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 850 ℃, and keeping the temperature for 60 min; c. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising furnace temperature to 1050 ℃, and keeping the temperature for 60 min; d. and (2) partial pressure sintering: introducing nitrogen, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then reducing the temperature of the furnace to 900 ℃; e. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃; step five, reduction and sintering by argon gas: and (3) placing the defective sintered part in the fourth step into the sintering furnace in the fourth step for argon reduction sintering to obtain a compact sintered part, which comprises the following specific steps: f. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min; g. partial pressure sintering: introducing argon, increasing partial pressure sintering pressure, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then reducing the furnace temperature to 1050 ℃; h. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃; step six, secondary sintering and nitriding: and (4) placing the compact sintered part prepared in the fifth step into the sintering furnace of the fourth step for secondary nitriding sintering to prepare a high-nitrogen nickel-free stainless steel product with stable size, and the specific steps are as follows: i. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min; j. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising furnace temperature to 1200 ℃, and keeping the temperature for 60 min; then reducing the furnace temperature to 1050 ℃; k. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃; and seventhly, carrying out solution treatment on the product to remove chromium nitride precipitates in the product. According to the invention, after the sintering defective product is subjected to Ar reduction, secondary sintering nitridation is carried out, and the sintering is qualified, so that the rejection rate is greatly reduced, the cost is reduced, and large-scale production can be realized.
Detailed Description
The present invention will be described below with reference to specific embodiments.
A high-nitrogen nickel-free stainless steel sintering process comprises the following steps:
step one, preparing a high-nitrogen nickel-free stainless steel feed: mixing high-nitrogen nickel-free stainless steel powder and a binder according to a ratio of 8:1, uniformly mixing, and putting the obtained mixture into a feeding crusher to prepare granular feed with uniform size;
step two, injection molding: molding the feed obtained in the step one in an injection molding machine to obtain an injection blank with an expected structure;
step three, degreasing: placing the injection blank obtained in the step two on a special ceramic jig, and degreasing the injection blank by using a special degreasing furnace to obtain a degreased part;
step four, sintering and nitriding: and (3) putting the degreased part prepared in the step three into a sintering furnace for nitriding and sintering to prepare the high-nitrogen nickel-free stainless steel sintered part, which comprises the following specific steps:
a. negative pressure degreasing: introducing nitrogen, heating the furnace to 850 ℃, and removing the binder which is not completely removed in the third step;
b. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 850 ℃, and keeping the temperature for 60 min;
c. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising the furnace temperature to 1050 ℃, and keeping the temperature for 60min, wherein the step is to prevent ferrite in the product from being left, so that the magnetic conductivity of the product is out of tolerance;
d. and (2) partial pressure sintering: introducing nitrogen, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then the furnace temperature is reduced to 900 ℃, and the product is sintered and compacted in the step;
e. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
step five, reduction and sintering by argon gas: and (3) placing the defective sintered part in the fourth step into the sintering furnace in the fourth step for argon reduction sintering to obtain a compact sintered part, which comprises the following specific steps:
f. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min;
g. partial pressure sintering: introducing argon, increasing partial pressure sintering pressure, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then reducing the furnace temperature to 1050 ℃;
h. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
step six, secondary sintering and nitriding: and (4) placing the compact sintered part prepared in the fifth step into the sintering furnace of the fourth step for secondary nitriding sintering to prepare a high-nitrogen nickel-free stainless steel product with stable size, and the specific steps are as follows:
i. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min;
j. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising furnace temperature to 1200 ℃, and keeping the temperature for 60 min; then reducing the furnace temperature to 1050 ℃;
k. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
and step seven, carrying out solution treatment on the product to remove chromium nitride precipitates in the product, wherein the existence of the chromium nitride precipitates in the step can reduce the antirust performance of the product, and the antirust capacity of chromium element disappears when the chromium element exists in the form of chromium nitride, so that after the stainless steel is sintered and nitrided, the solution annealing treatment in the step seven is mostly required to be added to remove the chromium nitride precipitates.
Further, the nitrogen content of the high-nitrogen nickel-free stainless steel feed in the step one is less than 0.3 percent.
Furthermore, the nitrogen content of the dense sintered part obtained in the fifth step is less than 0.5%.
Further, the nitrogen content of the six-dimensionally stable high-nitrogen nickel-free stainless steel product of step six is greater than 0.65%.
The invention can prepare the high-nitrogen nickel-free stainless steel with stable size under the condition of not influencing the material performance, thereby improving the process yield; and reducing and sintering the primary sintering defective products, and nitriding for the second time to obtain the high-nitrogen nickel-free stainless steel with expected size, so that the process rejection rate is greatly reduced, and the cost is effectively reduced.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (4)
1. A high-nitrogen nickel-free stainless steel sintering process is characterized by comprising the following steps:
step one, preparing a high-nitrogen nickel-free stainless steel feed: mixing high-nitrogen nickel-free stainless steel powder and a binder according to a ratio of 8:1, uniformly mixing, and putting the obtained mixture into a feeding crusher to prepare granular feed with uniform size;
step two, injection molding: molding the feed obtained in the step one in an injection molding machine to obtain an injection blank with an expected structure;
step three, degreasing: placing the injection blank obtained in the step two on a special ceramic jig, and degreasing the injection blank by using a special degreasing furnace to obtain a degreased part;
step four, sintering and nitriding: and (3) putting the degreased part prepared in the step three into a sintering furnace for nitriding and sintering to prepare the high-nitrogen nickel-free stainless steel sintered part, which comprises the following specific steps:
a. negative pressure degreasing: introducing nitrogen, and heating the furnace to 850 ℃;
b. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 850 ℃, and keeping the temperature for 60 min;
c. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising furnace temperature to 1050 ℃, and keeping the temperature for 60 min;
d. and (2) partial pressure sintering: introducing nitrogen, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then reducing the temperature of the furnace to 900 ℃;
e. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
step five, reduction and sintering by argon gas: and (3) placing the defective sintered part in the fourth step into the sintering furnace in the fourth step for argon reduction sintering to obtain a compact sintered part, which comprises the following specific steps:
f. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min;
g. partial pressure sintering: introducing argon, increasing partial pressure sintering pressure, raising the furnace temperature to 1240 ℃, and keeping the temperature for 210 min; then reducing the furnace temperature to 1050 ℃;
h. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
step six, secondary sintering and nitriding: and (4) placing the compact sintered part prepared in the fifth step into the sintering furnace of the fourth step for secondary nitriding sintering to prepare a high-nitrogen nickel-free stainless steel product with stable size, and the specific steps are as follows:
i. vacuum internal combustion: vacuumizing the sintering furnace, keeping the furnace temperature at 1050 ℃, and keeping the temperature for 210 min;
j. partial pressure sintering: introducing nitrogen, increasing partial pressure sintering pressure, raising furnace temperature to 1200 ℃, and keeping the temperature for 60 min; then reducing the furnace temperature to 1050 ℃;
k. forced cooling: introducing nitrogen, increasing the pressure, and rapidly cooling the furnace temperature to 60 ℃;
and seventhly, carrying out solution treatment on the product to remove chromium nitride precipitates in the product.
2. The sintering process of high-nitrogen nickel-free stainless steel according to claim 1, characterized in that: the nitrogen content of the high-nitrogen nickel-free stainless steel feed in the step one is less than 0.3 percent.
3. The sintering process of high-nitrogen nickel-free stainless steel according to claim 1, characterized in that: and fifthly, the nitrogen content of the dense sintered part obtained in the fifth step is less than 0.5%.
4. The sintering process of high-nitrogen nickel-free stainless steel according to claim 1, characterized in that: the nitrogen content of the six-dimensionally stable high-nitrogen nickel-free stainless steel product is greater than 0.65%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113502428A (en) * | 2021-06-23 | 2021-10-15 | 华南理工大学 | Method for preparing high-nitrogen nickel-free austenitic stainless steel and product thereof |
| CN113547119A (en) * | 2021-07-20 | 2021-10-26 | 东莞市华研新材料科技有限公司 | MIM316 sintering process |
| CN113732287A (en) * | 2021-09-13 | 2021-12-03 | 东莞市环力智能科技有限公司 | Non-magnetic sintering process for 17-4 products |
| CN114082950A (en) * | 2021-11-04 | 2022-02-25 | 金上晋科技(东莞)有限公司 | Method for improving mechanical property of SUS630 stainless steel injection molding finished product |
| CN114182178A (en) * | 2021-12-09 | 2022-03-15 | 广州金南磁性材料有限公司 | High-nitrogen nickel-free austenitic stainless steel and preparation method and application thereof |
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| CN111451507A (en) * | 2020-05-27 | 2020-07-28 | 江苏省海洋资源开发研究院(连云港) | Near-net forming method of high-nitrogen nickel-free austenitic stainless steel |
| CN111621705A (en) * | 2020-06-19 | 2020-09-04 | 深圳市泛海统联精密制造股份有限公司 | Preparation method of nickel-free duplex stainless steel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113502428A (en) * | 2021-06-23 | 2021-10-15 | 华南理工大学 | Method for preparing high-nitrogen nickel-free austenitic stainless steel and product thereof |
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| CN113732287B (en) * | 2021-09-13 | 2024-05-28 | 东莞市环力智能科技有限公司 | Nonmagnetic sintering process for 17-4 product |
| CN114082950A (en) * | 2021-11-04 | 2022-02-25 | 金上晋科技(东莞)有限公司 | Method for improving mechanical property of SUS630 stainless steel injection molding finished product |
| CN114082950B (en) * | 2021-11-04 | 2024-04-16 | 金上晋科技(东莞)有限公司 | Method for improving mechanical properties of SUS630 stainless steel injection molding finished product |
| CN114182178A (en) * | 2021-12-09 | 2022-03-15 | 广州金南磁性材料有限公司 | High-nitrogen nickel-free austenitic stainless steel and preparation method and application thereof |
| CN114182178B (en) * | 2021-12-09 | 2022-10-18 | 广州金南磁性材料有限公司 | Preparation method and application of high-nitrogen nickel-free austenitic stainless steel |
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| CN112517911B (en) | 2023-05-16 |
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