CN108273989B - High-temperature heat treatment method for preventing metal alloy fine powder from caking - Google Patents
High-temperature heat treatment method for preventing metal alloy fine powder from caking Download PDFInfo
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- CN108273989B CN108273989B CN201711405800.1A CN201711405800A CN108273989B CN 108273989 B CN108273989 B CN 108273989B CN 201711405800 A CN201711405800 A CN 201711405800A CN 108273989 B CN108273989 B CN 108273989B
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- temperature
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 54
- 239000000843 powder Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910001092 metal group alloy Inorganic materials 0.000 title claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 238000005054 agglomeration Methods 0.000 claims description 6
- 230000002776 aggregation Effects 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 12
- 239000000956 alloy Substances 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000000630 rising effect Effects 0.000 abstract 2
- 239000002184 metal Substances 0.000 description 10
- 229910001111 Fine metal Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
- C21D1/32—Soft annealing, e.g. spheroidising
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D11/00—Process control or regulation for heat treatments
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
- B22F2201/11—Argon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The high temperature heat treatment method for preventing metal alloy fine powder from caking is simple, low in cost and suitable for mass production. Placing the alloy fine powder to be treated in an atmosphere rotary furnace, rotating the rotary furnace at a certain rotating speed in the temperature rising process, then rising to the required heat treatment temperature, circularly performing positive and negative rotation at fixed time intervals in a high-temperature area, and then performing the specified heat treatment process, wherein the applicable heat treatment temperature is below 950 ℃.
Description
Technical Field
The invention relates to a method for the anti-caking treatment of fine metal powders, in particular during high-temperature heat treatment.
Background
Metal powder is a widely used raw material in the engineering field. The powder required in spraying, laser cladding and 3D printing has the characteristics of small size, large specific surface area, good fluidity and the like, but different application directions have different requirements on the performance of the powder, such as the requirement on particle size distribution, the requirement on sphericity and the requirement on hardness and the like.
In many cases, the powder material needs to be pre-treated before use, depending on the application conditions. If the powder is required to be dried before use, the treatment is relatively simple and only involves temperature and holding time. However, in certain particularly demanding applications, high temperature heat treatment of the metal powder is required to obtain coarser grains or other specific textures and properties, such as a softening annealing treatment. The metal powder generally has a high-temperature agglomeration phenomenon in the high-temperature heat treatment process, namely the high-temperature sintering which is often called. Therefore, it is of great practical significance to find a suitable treatment method to solve the problem of anti-caking of the metal powder during the high temperature heat treatment.
Disclosure of Invention
The invention aims to provide a high-temperature heat treatment method for preventing metal powder from caking, which is simple in process, low in cost and suitable for mass production, aiming at the problems in the existing heat treatment of metal fine spherical alloy powder. The temperature of the anti-caking high-temperature heat treatment method of the present invention is specifically a high-temperature heat treatment at 950 ℃ or lower.
According to one aspect of the present invention, there is provided a high temperature heat treatment method for preventing agglomeration of fine metal alloy powder, comprising the steps of:
(1) placing metal powder to be treated in an atmosphere rotary furnace, and rotating the rotary furnace;
(2) heating the rotary furnace to a temperature between 100 ℃ and 200 ℃ and preserving the heat for more than 2 hours;
(3) after the temperature of the rotary furnace is raised to a temperature point between 500 ℃ and 600 ℃, the rotary furnace is circularly rotated in a positive and negative way at a fixed time interval;
(4) and finally carrying out a further heat treatment process.
Advantageously, in the step (1), high-purity argon is used for replacing the atmosphere in the furnace, and the furnace is vacuumized and kept in an ultimate vacuum state.
Advantageously, in step (2), the extreme vacuum state is maintained.
Advantageously, in step (3), the rotary furnace is heated to a temperature between 500 ℃ and 600 ℃ and then is filled with a protective atmosphere after heat preservation.
Advantageously, the rotary kiln in step (1) is rotated at a speed of 4 to 7 rpm.
Advantageously, the high temperature heat treatment in step (4) is a softening annealing treatment.
Advantageously, the further heat treatment process in step (4) is specifically: slowly heating the rotary furnace to a certain temperature point between 700 and 950 ℃, preserving the temperature for 15 hours, then cooling the rotary furnace to 600 ℃ at a certain cooling speed, cooling the rotary furnace to room temperature, and discharging the powder out of the rotary furnace.
Advantageously, the further heat treatment process in step (4) is specifically: slowly heating the rotary furnace to 860 ℃, preserving heat for 13-15 hours, then cooling to 600 ℃ at the cooling speed of 10 ℃ per hour, cooling to room temperature, and discharging the powder from the furnace.
According to another aspect of the present invention, there is provided a high temperature heat treatment method for preventing agglomeration of fine metal alloy powder, comprising the following steps:
(1) placing the metal powder to be treated in an atmosphere rotary furnace, replacing the atmosphere in the furnace after closing the furnace (the times can be determined according to the requirement), and finally keeping the ultimate vacuum state;
(2) heating the equipment to a temperature point between 100 ℃ and 200 ℃ for heat preservation for more than 2 hours, and keeping a limit vacuum state;
(3) heating the equipment to a temperature point between 500 ℃ and 600 ℃, preserving heat, filling protective atmosphere, and circularly performing positive and negative rotation of the rotary furnace at a fixed time interval;
(4) and (4) carrying out a corresponding heat treatment process after the heat preservation in the step (3) is finished.
In the step (1), the equipment adopts a special atmosphere rotary furnace, and the protective atmosphere is high-purity argon. By adopting the scheme to carry out the heat treatment, the temperature of the heat treatment can be below 950 ℃, and the holding time of the heat treatment can be within 15 hours (for example, 860 ℃ and above). Advantageously, the problem of agglomeration of the alloy powder during high temperature heat treatment is thoroughly solved by precise gradient control of the temperature of the alloy fine powder in combination with rotational treatment.
Detailed Description
In the case of the example 1, the following examples are given,
the invention provides a high-temperature heat treatment method for preventing metal alloy fine powder from caking. The method preferably comprises the steps of:
(1) placing metal powder to be treated in an atmosphere rotary furnace, and rotating the rotary furnace;
(2) heating the rotary furnace to a temperature between 100 ℃ and 200 ℃ and preserving the heat for more than 2 hours;
(3) after the temperature of the rotary furnace is raised to a temperature point between 500 ℃ and 600 ℃, the rotary furnace is circularly rotated in a positive and negative way at a fixed time interval;
(4) and finally carrying out a further heat treatment process.
Advantageously, in the step (1), high-purity argon is used for replacing the atmosphere in the furnace, and the furnace is vacuumized and kept in an ultimate vacuum state.
Advantageously, in step (2), the extreme vacuum state is maintained.
Advantageously, in step (3), the rotary furnace is heated to a temperature between 500 ℃ and 600 ℃ and then is filled with a protective atmosphere after heat preservation.
Advantageously, the rotary kiln in step (1) is rotated at a speed of 4 to 7 rpm.
Advantageously, the high temperature heat treatment in step (4) is a softening annealing treatment.
Advantageously, the further heat treatment process in step (4) is specifically: slowly heating the rotary furnace to a certain temperature point between 700 and 950 ℃, preserving the temperature for 15 hours, then cooling the rotary furnace to 600 ℃ at a certain cooling speed, cooling the rotary furnace to room temperature, and discharging the powder out of the rotary furnace.
Advantageously, the further heat treatment process in step (4) is specifically: slowly heating the rotary furnace to 860 ℃, preserving heat for 13-15 hours, then cooling to 600 ℃ at the cooling speed of 10 ℃ per hour, cooling to room temperature, and discharging the powder from the furnace.
Advantageously, the protective atmosphere charged in step (3) is to be high-purity argon and high-purity hydrogen. The proportion of the high-purity argon gas and the high-purity hydrogen gas is preferably 9: 1. the pressure of the charge is preferably slightly less than one atmosphere. Advantageously, the incubation time in step (3) is more than 1 hour.
Advantageously, the hardness of the alloy fine powder is reduced to HV 175-185, such as HV 180. It is understood that the powder involved in the present invention is a fine spherical metal powder having an average diameter of 150 μm or less, and the provided anti-caking high-temperature heat treatment method is simple, low-cost, and suitable for mass production, and the applicable heat treatment temperature is 950 ℃ or less.
Example 2 (taking H13 powder, spherical powder with an average diameter below 100 μm as an example):
taking 150 kg of powder, placing the powder in an atmosphere rotary furnace, sealing the furnace, pumping to limit vacuum, then filling high-purity argon to atmospheric pressure, pumping to limit vacuum, repeating the steps for two to three times, and finally keeping the limit vacuum state.
Rotating the equipment at 5-7 rpm, heating the equipment to 150 ℃, preserving the heat for 3-5 hours, and keeping the ultimate vacuum state; the apparatus was further warmed to 500 ℃ and incubated for 1 hour, during which time the limiting vacuum was maintained. When the heat preservation is about to be finished, high-purity argon and high-purity hydrogen (the ratio is 9: 1) are filled to be slightly lower than one atmosphere, and the equipment is circularly rotated in a positive and negative mode at intervals of every half hour.
Slowly heating the equipment to 860 ℃, preserving heat for 13-15 hours, then cooling to 600 ℃ at the cooling speed of 10 ℃ per hour, then cooling to room temperature, and discharging the powder from the furnace.
The high-temperature heat treatment is softening annealing treatment of the H13 material, and finally can reduce the powder hardness of H13 to HV 180.
It can be understood that the present invention is carried out by placing the alloy fine powder to be processed in an atmosphere rotary furnace, rotating the rotary furnace at a certain rotation speed during the temperature rise, then raising the temperature to the desired heat treatment temperature, and carrying out a regular and reverse rotation cycle at fixed time intervals in a high temperature region, and then carrying out the specified heat treatment process. By finely controlling and skillfully processing the temperature and rotation of the alloy fine powder, the problem of agglomeration of the alloy powder in the high-temperature heat treatment process is thoroughly solved, the performance parameters (such as particle size distribution, sphericity and hardness) of the alloy powder are improved, and the accurate control of the performance of the alloy powder can be realized.
Claims (8)
1. A high-temperature heat treatment method for preventing agglomeration of metal alloy fine powder is characterized by comprising the following steps of:
1) placing the metal alloy fine powder to be treated in an atmosphere rotary furnace, and rotating the atmosphere rotary furnace;
2) heating the atmosphere rotary furnace to a temperature point of 100 ~ 200 ℃ and preserving heat for more than 2 hours;
3) after the temperature of the atmosphere rotary furnace is raised to a temperature point between 500 and 500 ~ 600 ℃, the atmosphere rotary furnace is maintained at a fixed time interval and is rotated in a positive and negative direction;
4) and finally carrying out a further heat treatment process.
2. The method of claim 1, wherein the atmosphere in the furnace is replaced with high purity argon gas in step 1), and the furnace is evacuated and maintained at an ultimate vacuum.
3. The method of claim 2, wherein in step 2), the extreme vacuum condition is maintained.
4. The method of claim 3, wherein in step 3), the atmosphere rotary furnace is heated to a temperature between 500 ℃ and 500 ~ 600 ℃ and then is filled with protective atmosphere after heat preservation.
5. The method according to any one of claims 1 to 4, wherein the rotation speed of the rotary atmosphere furnace in step 1) is 4 to 7 rpm.
6. A method according to any of claims 1-4, characterized in that the heat treatment in step 4) is a softening annealing treatment.
7. The method according to any of claims 1 to 4, characterized in that the further heat treatment in step 4) is in particular: slowly heating the atmosphere rotary furnace to a certain temperature point between 700 and 950 ℃, preserving the temperature for 15 hours, then cooling the temperature to 600 ℃ at a certain cooling speed, cooling the furnace to room temperature, and discharging the powder out of the furnace.
8. The method according to any of claims 1 to 4, characterized in that the further heat treatment in step 4) is in particular: slowly heating the atmosphere rotary furnace to 860 ℃, preserving heat for 13-15 hours, then cooling to 600 ℃ at the cooling speed of 10 ℃ per hour, cooling to room temperature, and discharging the powder.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711405800.1A CN108273989B (en) | 2017-12-22 | 2017-12-22 | High-temperature heat treatment method for preventing metal alloy fine powder from caking |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711405800.1A CN108273989B (en) | 2017-12-22 | 2017-12-22 | High-temperature heat treatment method for preventing metal alloy fine powder from caking |
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| CN108273989A CN108273989A (en) | 2018-07-13 |
| CN108273989B true CN108273989B (en) | 2020-01-21 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110499482A (en) * | 2019-10-11 | 2019-11-26 | 辽宁工业大学 | A kind of high-temperature heat treatment method of nickel based metal alloy powder |
| CN111750665A (en) * | 2020-07-28 | 2020-10-09 | 赣州鼎盛炉业有限公司 | High-efficiency energy-saving rotary furnace |
| CN111750664A (en) * | 2020-07-28 | 2020-10-09 | 赣州鼎盛炉业有限公司 | Rotary furnace with heat insulating plate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52156124A (en) * | 1976-06-22 | 1977-12-26 | Kawasaki Steel Co | Production of nonanisotropic silicon steel sheets |
| US4272285A (en) * | 1979-07-12 | 1981-06-09 | Tdk Electronics Co., Ltd. | Process for producing magnetic metal powders |
| CN1305399A (en) * | 1998-05-22 | 2001-07-25 | 卡伯特公司 | Method to agglomerate metal particles and metal particles having improved properties |
| CN101254542A (en) * | 2008-04-22 | 2008-09-03 | 重庆铸信粉末冶金有限责任公司 | Iron-based brassiness powder metallurgy material and preparation |
| CN106637013A (en) * | 2016-10-28 | 2017-05-10 | 机械科学研究总院先进制造技术研究中心 | Thermal treatment method capable of enhancing high temperature strength of Ti2AlNb-based alloy |
-
2017
- 2017-12-22 CN CN201711405800.1A patent/CN108273989B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52156124A (en) * | 1976-06-22 | 1977-12-26 | Kawasaki Steel Co | Production of nonanisotropic silicon steel sheets |
| US4272285A (en) * | 1979-07-12 | 1981-06-09 | Tdk Electronics Co., Ltd. | Process for producing magnetic metal powders |
| CN1305399A (en) * | 1998-05-22 | 2001-07-25 | 卡伯特公司 | Method to agglomerate metal particles and metal particles having improved properties |
| CN101254542A (en) * | 2008-04-22 | 2008-09-03 | 重庆铸信粉末冶金有限责任公司 | Iron-based brassiness powder metallurgy material and preparation |
| CN106637013A (en) * | 2016-10-28 | 2017-05-10 | 机械科学研究总院先进制造技术研究中心 | Thermal treatment method capable of enhancing high temperature strength of Ti2AlNb-based alloy |
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| CN108273989A (en) | 2018-07-13 |
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Effective date of registration: 20211101 Address after: 450001 100m North West of the intersection of Chemical Road and Xiangpu Road, high tech Zone, Zhengzhou City, Henan Province Patentee after: China Machinery New Material Research Institute (Zhengzhou) Co.,Ltd. Address before: 100083 No. 18 clear road, Haidian District, Beijing Patentee before: BEIJING NATIONAL INNOVATION INSTITUTE OF LIGHTWEIGHT Ltd. |
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Denomination of invention: A high temperature heat treatment method for preventing caking of metal alloy micro powder Effective date of registration: 20220628 Granted publication date: 20200121 Pledgee: Bank of China Zhengzhou branch of Limited by Share Ltd. culture Pledgor: China Machinery New Material Research Institute (Zhengzhou) Co.,Ltd. Registration number: Y2022980009271 |
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Date of cancellation: 20230728 Granted publication date: 20200121 Pledgee: Bank of China Zhengzhou branch of Limited by Share Ltd. culture Pledgor: China Machinery New Material Research Institute (Zhengzhou) Co.,Ltd. Registration number: Y2022980009271 |
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Denomination of invention: A High Temperature Heat Treatment Method for Preventing Agglomeration of Metal Alloy Fine Powder Effective date of registration: 20230807 Granted publication date: 20200121 Pledgee: Bank of China Zhengzhou branch of Limited by Share Ltd. culture Pledgor: China Machinery New Material Research Institute (Zhengzhou) Co.,Ltd. Registration number: Y2023980050871 |
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Granted publication date: 20200121 Pledgee: Bank of China Zhengzhou branch of Limited by Share Ltd. culture Pledgor: China Machinery New Material Research Institute (Zhengzhou) Co.,Ltd. Registration number: Y2023980050871 |