CN108273989A - A kind of high-temperature heat treatment method of metal alloy attritive powder anti-caking - Google Patents
A kind of high-temperature heat treatment method of metal alloy attritive powder anti-caking Download PDFInfo
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- CN108273989A CN108273989A CN201711405800.1A CN201711405800A CN108273989A CN 108273989 A CN108273989 A CN 108273989A CN 201711405800 A CN201711405800 A CN 201711405800A CN 108273989 A CN108273989 A CN 108273989A
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- Prior art keywords
- heat treatment
- temperature
- caking
- rotary furnace
- treatment method
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- 239000000843 powder Substances 0.000 title claims abstract description 53
- 238000010438 heat treatment Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910001092 metal group alloy Inorganic materials 0.000 title claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 14
- 238000004321 preservation Methods 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 abstract description 9
- 239000000956 alloy Substances 0.000 abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction 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
A kind of high-temperature heat treatment method of metal alloy attritive powder anti-caking, involved powder be average diameter in 150 μm of superfine spherical metal powders below, the high-temperature heat treatment method of the anti-caking provided is simple, at low cost, is suitable for producing in enormous quantities.Pending micro-alloy powder is placed in atmosphere rotary furnace, in temperature-rise period, make rotary furnace with certain rotational speed, then it is raised to required heat treatment temperature, and time interval positive and negative rotation cycle is fixed in high-temperature region and carries out, then specified heat treatment process is carried out, the heat treatment temperature being applicable in is 950 DEG C or less.
Description
Technical field
The present invention relates to refining metallic powders, the processing side of the anti-caking of metal powder especially in high-temperature heat treatment process
Method.
Background technology
Metal powder is that have widely applied raw material in a kind of engineering field.In spraying, laser melting coating and 3D printing
In required powder have the characteristics that small size, large specific surface area, good fluidity, but be different application direction to powder
Performance has different requirements, such as size distribution requirements, sphericity requirement and hardness requirement etc..
Dusty material is required for processing before being carried out according to application conditions before use in many cases,.Make as
With preceding needing to be dried processing to powder, this processing is relatively simple, pertains only to temperature and soaking time.But at certain
The application scenario of a little particular/special requirements needs to carry out high-temperature heat treatment to metal powder, to obtain compared with coarse grain or other specific groups
It knits and performance, as soft annealing is handled.And metal powder generally existing caking at high temperature phenomenon in high-temperature heat treatment process, also
It is the high temperature sintering that we often say.Therefore, seek suitable processing method to solve metal powder in high-temperature heat treatment process
Anti-caking problem have important practical significance.
Invention content
It is an object of the invention to be directed to the above problem present in existing metal superfine alloyed spherical powder heat treatment,
Simple process and low cost is provided, a kind of high-temperature heat treatment method of the anti-caking for the metal powder produced in enormous quantities is suitable for.It needs
It is noted that the temperature of anti-caking high-temperature heat treatment method of the present invention specifically refers at 950 DEG C of high warms below
Reason.
According to an aspect of the present invention, a kind of high-temperature heat treatment method of metal alloy attritive powder anti-caking is provided,
It is characterized in that including the following steps：
（1）Pending metal powder is placed in atmosphere rotary furnace, rotary furnace is made to rotate；
（2）Rotary furnace is warming up to the heat preservation that the temperature spot between 100-200 DEG C carries out 2 hours or more；
（3）After rotary furnace is warming up to the heat preservation of the temperature spot between 500-600 DEG C, make rotary furnace in Fixed Time Interval positive and negative rotation
Cycle carries out；
（4）Finally carry out further heat treatment process.
Advantageously, step（1）It is middle that furnace atmosphere is replaced using high-purity argon gas, it vacuumizes and keeps end vacuum state.
Advantageously, step（2）In, keep end vacuum state.
Advantageously, step（3）In, it is filled with protection gas after rotary furnace is warming up to the heat preservation of the temperature spot between 500-600 DEG C
Atmosphere.
Advantageously, step（1）The velocity of rotation of middle rotary furnace is 4-7 revs/min.
Advantageously, step（4）In high-temperature heat treatment be soft annealing processing.
Advantageously, step（4）In further heat treatment process be specially：Rotary furnace is to slowly warm up to 700-950 DEG C
Between some temperature spot and keep the temperature 15 hours within, after then dropping to 600 DEG C with certain cooling rate furnace cooling arrive room temperature, general
Powder is come out of the stove.
Advantageously, step（4）In further heat treatment process be specially：Rotary furnace is to slowly warm up to 860 DEG C and is protected
13-15 hours warm, furnace cooling comes out of the stove powder to room temperature after then dropping to 600 DEG C with 10 DEG C per hour of cooling rate.
According to a further aspect of the invention, a kind of high-temperature heat treatment side of metal alloy attritive powder anti-caking is additionally provided
Method is as follows：
（1）Pending metal powder is placed in atmosphere rotary furnace, enclosed furnace rear substitution furnace atmosphere（Number can be according to need
To determine）, finally keep end vacuum state；
（2）Equipment is warming up to the temperature spot between 100-200 DEG C and carries out heat preservations in 2 hours or more, and keeps end vacuum shape
State；
（3）It is filled with protective atmosphere after equipment is warming up to the heat preservation of the temperature spot between 500-600 DEG C, and makes rotary furnace when fixed
Between interval positive and negative rotation cycle carry out；
（4）In step（3）Corresponding heat treatment process is carried out after heat preservation.
In step（1）In, the equipment uses specific atmosphere rotary furnace, and protective atmosphere is high-purity argon gas.Using this
Scheme is heat-treated, and the temperature of heat treatment can be at 950 DEG C hereinafter, the soaking time of heat treatment can be within 15 hours
（Such as 860 DEG C or more）.Advantageously, by combining rotation to handle the exact gradient control of the micro-alloy powder temperature,
Thoroughly solve agglomeration problems of the alloy powder in high-temperature heat treatment process.
Specific implementation mode
Embodiment 1,
The present invention provides a kind of high-temperature heat treatment methods of metal alloy attritive powder anti-caking.This method preferably include as
Lower step：
（1）Pending metal powder is placed in atmosphere rotary furnace, rotary furnace is made to rotate；
（2）Rotary furnace is warming up to the heat preservation that the temperature spot between 100-200 DEG C carries out 2 hours or more；
（3）After rotary furnace is warming up to the heat preservation of the temperature spot between 500-600 DEG C, make rotary furnace in Fixed Time Interval positive and negative rotation
Cycle carries out；
（4）Finally carry out further heat treatment process.
Advantageously, step（1）It is middle that furnace atmosphere is replaced using high-purity argon gas, it vacuumizes and keeps end vacuum state.
Advantageously, step（2）In, keep end vacuum state.
Advantageously, step（3）In, it is filled with protection gas after rotary furnace is warming up to the heat preservation of the temperature spot between 500-600 DEG C
Atmosphere.
Advantageously, step（1）The velocity of rotation of middle rotary furnace is 4-7 revs/min.
Advantageously, step（4）In high-temperature heat treatment be soft annealing processing.
Advantageously, step（4）In further heat treatment process be specially：Rotary furnace is to slowly warm up to 700-950 DEG C
Between some temperature spot and keep the temperature 15 hours within, after then dropping to 600 DEG C with certain cooling rate furnace cooling arrive room temperature, general
Powder is come out of the stove.
Advantageously, step（4）In further heat treatment process be specially：Rotary furnace is to slowly warm up to 860 DEG C and is protected
13-15 hours warm, furnace cooling comes out of the stove powder to room temperature after then dropping to 600 DEG C with 10 DEG C per hour of cooling rate.
Advantageously, step（3）In the protective atmosphere that is filled with wait for as high-purity argon gas and high-purity hydrogen.High-purity argon gas and High Purity Hydrogen
The ratio of gas is preferably ratio 9：1.The pressure being filled with a preferably slightly below atmospheric pressure.
Advantageously, step（3）In soaking time be 1 hour or more.
Advantageously, the hardness of micro-alloy powder is reduced to HV 175-185, such as HV 180.It is understood that this
Involved powder is average diameter in 150 μm of superfine spherical metal powders below, the height of the anti-caking provided in invention
It is simple to warm processing method, it is at low cost, it is suitable for producing in enormous quantities, the heat treatment temperature being applicable in is 950 DEG C or less.
Embodiment 2（With H13 powder, average diameter in 100 μm of spherical powders below, for）：
150 kg of powder is taken, is placed in atmosphere rotary furnace, enclosed furnace is first evacuated to end vacuum, is then charged with high-purity argon gas extremely
Atmospheric pressure, then it is evacuated to end vacuum, two to three times repeatedly, finally keeps end vacuum state.
Equipment is set to be rotated with 5-7 revs/min, equipment, which is warming up to 150 DEG C, keeps the temperature 3-5 hours, and keeps end vacuum state；After
It is continuous that equipment is warming up to 500 DEG C and carries out heat preservation in 1 hour, holding end vacuum state during this.It is filled when heat preservation closes to an end
Enter high-purity argon gas and high-purity hydrogen（Ratio 9：1）To a slightly below atmospheric pressure, at this time by equipment using per half an hour as interval
Positive and negative rotation cycle carries out.
Equipment is to slowly warm up to 860 DEG C and keeps the temperature 13-15 hours, is then dropped to 10 DEG C per hour of cooling rate
Furnace cooling comes out of the stove powder to room temperature after 600 DEG C.
The high-temperature heat treatment is that the soft annealing of H13 materials is handled, and finally can the powder hardness of H13 be reduced to HV 180
Up and down.
It is understood that the present invention is being heated up by the way that pending micro-alloy powder to be placed in atmosphere rotary furnace
In the process, make rotary furnace with certain rotational speed, be then raised to required heat treatment temperature, and be fixed in high-temperature region
Time interval positive and negative rotation cycle carries out, and then carries out specified heat treatment process.By temperature to the micro-alloy powder and
The precise controlling of rotation and manipulative, thoroughly solves agglomeration problems of the alloy powder in high-temperature heat treatment process, improves
The performance parameter of alloy powder（Such as size distribution, sphericity, hardness）, it can be achieved that the accurate control to alloy powder performance
System.
Claims (8)
1. a kind of high-temperature heat treatment method of metal alloy attritive powder anti-caking, it is characterised in that include the following steps：
（1）Pending metal powder is placed in atmosphere rotary furnace, rotary furnace is made to rotate；
（2）Rotary furnace is warming up to the heat preservation that the temperature spot between 100 ~ 200 DEG C carries out 2 hours or more；
（3）After rotary furnace is warming up to the heat preservation of the temperature spot between 500 ~ 600 DEG C, make rotary furnace in Fixed Time Interval positive and negative rotation
Cycle carries out；
（4）Finally carry out further heat treatment process.
2. a kind of high-temperature heat treatment method of metal alloy powders anti-caking as described in claim 1, it is characterised in that step（1）
It is middle that furnace atmosphere is replaced using high-purity argon gas, it vacuumizes and keeps end vacuum state.
3. a kind of high-temperature heat treatment method of metal alloy powders anti-caking as claimed in claim 2, it is characterised in that step（2）
In, keep end vacuum state.
4. a kind of high-temperature heat treatment method of metal alloy powders anti-caking as claimed in claim 3, it is characterised in that step（3）
In, it is filled with protective atmosphere after rotary furnace is warming up to the heat preservation of the temperature spot between 500 ~ 600 DEG C.
5. a kind of high-temperature heat treatment method of metal alloy powders anti-caking, feature exist as described in claim any one of 1-4
In step（1）The velocity of rotation of middle rotary furnace is 4-7 revs/min.
6. a kind of high-temperature heat treatment method of metal alloy powders anti-caking, feature exist as described in claim any one of 1-4
In step（4）In high-temperature heat treatment be soft annealing processing.
7. a kind of high-temperature heat treatment method of metal alloy powders anti-caking, feature exist as described in claim any one of 1-4
In step（4）In further heat treatment process be specially：Some temperature rotary furnace being to slowly warm up between 700-950 DEG C
It puts and keeps the temperature within 15 hours, furnace cooling comes out of the stove powder to room temperature after then dropping to 600 DEG C with certain cooling rate.
8. a kind of high-temperature heat treatment method of metal alloy powders anti-caking, feature exist as described in claim any one of 1-4
In step（4）In further heat treatment process be specially：Rotary furnace is to slowly warm up to 860 DEG C and keeps the temperature 13-15 hours, so
Furnace cooling comes out of the stove powder to room temperature after dropping to 600 DEG C afterwards with 10 DEG C per hour of cooling rate.
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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 true CN108273989A (en) | 2018-07-13 |
| CN108273989B CN108273989B (en) | 2020-01-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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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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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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