CN110835673A - Method for preventing stainless steel from being oxidized during heat treatment - Google Patents
Method for preventing stainless steel from being oxidized during heat treatment Download PDFInfo
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- CN110835673A CN110835673A CN201911250224.7A CN201911250224A CN110835673A CN 110835673 A CN110835673 A CN 110835673A CN 201911250224 A CN201911250224 A CN 201911250224A CN 110835673 A CN110835673 A CN 110835673A
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- 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
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
-
- 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
- C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
- C21D1/70—Temporary coatings or embedding materials applied before or during heat treatment while heating or quenching
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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)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Heat Treatment Of Articles (AREA)
Abstract
The invention relates to a method for preventing stainless steel from being oxidized in heat treatment, which comprises the following steps: 1) preparing a tool, titanium chips and the like; 2) treating the parts before entering the furnace; 3) vacuum heat treatment process: loading the parts on the cleaned tool in the step 1), preventing nesting, stacking or matching, placing the parts in a manner of a layer of titanium chips and a layer of parts, laying a layer of titanium chips on the outermost layer of parts, and heating the parts in an effective working area; setting technological parameters, controlling the vacuum degree in the furnace to be less than or equal to 1.33 multiplied by 10‑1Pa, heating to 482 +/-14 ℃, preserving heat for at least 1 hour, refilling high-purity argon until the temperature in the furnace is cooled to be less than or equal to 371 ℃, stopping refilling argon, continuing cooling the part in the furnace, opening the door when the temperature reaches below 200 ℃, taking out the part, and air-cooling; 4) and (5) checking and packaging. The method is a method for efficiently and reliably suppressing the formation of an oxide of a component by burying the component with titanium dust as an auxiliary medium and performing heat treatment.
Description
Technical Field
The invention relates to a method for preventing stainless steel from being oxidized in heat treatment, belonging to the field of heat treatment.
Background
At present, the method for preventing stainless steel from being oxidized by heat treatment comprises the steps of coating an anti-oxidation protective coating on a part in the heat treatment process, and removing oxides by adopting sand blowing, acid washing or a mechanical method after the heat treatment, provided that the part does not exceed the dimensional tolerance in the drawing after the oxides are removed. Vacuum heat treatment is widely used in industry when it is considered to be an ideal, non-oxidizing, non-decarburizing, bright technique. However, in reality, because the parameters such as the vacuum degree and the vacuum inflation pressure are not properly selected, oxide layers with different degrees are formed on the surface of the part, or alloy elements are evaporated, so that the surface is depleted of the formed alloy elements.
Disclosure of Invention
The invention provides a method for preventing stainless steel from being oxidized in heat treatment, which uses titanium chips as an auxiliary medium to bury parts for heat treatment, thereby efficiently and reliably inhibiting the formation of part oxides.
In order to solve the above problems, the specific technical scheme of the invention is as follows: a method for preventing stainless steel from being oxidized by heat treatment, comprising the following steps:
1) preparing a tool, titanium chips and the like: manually cleaning the tool and the fixture by using acetone or alcohol, and drying; collecting titanium scraps Ti-6Al-4V, soaking and cleaning with acetone, then carrying out alkali cleaning, finally washing with water and drying; before each production, degassing titanium chips at a temperature not lower than the heating temperature of the part and under a vacuum degree in advance;
2) treating parts before entering the furnace: according to a part cleaning program, manually cleaning the part by using acetone or alcohol solvent, and cleaning the part before furnace installation by combining an alkali cleaning mode if necessary, wherein a water film on the surface of the part is ensured to be continuous in an alkali cleaning water washing process, and finally wiping the part dry or drying the part by using clean compressed air;
3) vacuum heat treatment process: loading the parts on the cleaned tool in the step 1), preventing nesting, stacking or matching, placing the parts in a manner of a layer of titanium chips and a layer of parts, laying a layer of titanium chips on the outermost layer of parts, and heating the parts in an effective working area; setting technological parameters, controlling the vacuum degree in the furnace to be less than or equal to 1.33 multiplied by 10-1Pa, heating to 482 +/-14 ℃, preserving heat for at least 1 hour, refilling high-purity argon until the temperature in the furnace is cooled to be less than or equal to 371 ℃, and stopping refilling argonContinuously cooling the parts in the furnace, opening the door when the temperature reaches below 200 ℃, taking out the parts, and cooling in the air;
4) and (3) inspection and packaging transfer: after the parts are taken out of the furnace, the parts are taken, placed and inspected by wearing clean white gloves, and the parts are packaged by polyethylene bags or kraft paper bags and then transferred to the next procedure.
The thickness of the part in the step 3) is less than or equal to 25mm, and when the thickness of the part is increased by 25mm, the heat preservation time is prolonged by 1 hour.
The method for preventing the stainless steel from being oxidized by heat treatment has the following advantages:
1. the stainless steel is one of the most widely applied structural materials for civil aviation, and the invention is suitable for all stainless steel components needing vacuum heat treatment and has wide application range;
2. the titanium chips are adopted to assist the heat treatment process, the search is not needed, only the chips are buried, the heat treatment time is adjusted according to the process specification requirement, and the operation is simple, convenient and reliable;
3. the formation of an oxide layer can be effectively reduced by adopting titanium chip-assisted vacuum heat treatment;
4. the consumption cost of protective coating caused by traditional heat treatment anti-oxidation treatment and the working hour and cost caused by sand blowing and mechanical removal are saved, and the method has good economic benefit.
Detailed Description
The solution idea of the invention is as follows: the degree of the oxide layer generated on the surface during the heat treatment of the stainless steel is determined by means of XPS (X-ray photoelectron spectroscopy) detection means. XPS detection is carried out by randomly selecting the test piece subjected to the heat treatment before and after the titanium chip assistance, and the oxygen content on the surface of the test piece is reduced from 47.76% to 30.89% after Ar gas is sputtered for 120s, which shows that the titanium chip assistance process method can effectively reduce the oxygen partial pressure in a furnace, thereby reducing the thickness of an oxide film on the surface of a part. The theory that titanium alloy and stainless steel are in the same potential grouping is combined, the principle that the affinity of titanium to oxygen is prior to aluminum and chromium is utilized, and a method of embedding titanium scraps is adopted, namely titanium is used as a sacrificial layer to protect parts, so that the formation of a heat treatment oxide layer is effectively inhibited or reduced. Through test piece and part tests and XPS detection verification, the method can effectively reduce the thickness of the oxide layer. After further passivation, the surface no longer has iridescence such as yellow, blue and the like. The method can effectively improve the appearance of the part and simultaneously provides a good surface state for the uniformity of the passivation film layer.
The implementation adopts precipitation hardening stainless steel joint parts, the material brand PH13-8Mo, the heat treatment state H1000, and the stress relief heat treatment process as an example, and further describes the patent process method of the invention, and the specific steps are as follows:
1) preparing a tool, titanium chips and the like: manually cleaning the tool and the fixture by using acetone or alcohol, and drying, wherein the cleaned surface is free from oil stains, fingerprints and residual solvents; collecting titanium scraps Ti-6Al-4V, soaking and cleaning with acetone, then alkaline cleaning (Isoprep 44# cleaning agent), and finally water (Cl)-Less than or equal to 30 ppm) washing and drying; before each production, the temperature of heating the parts is not lower than 482 +/-14 ℃ and the vacuum degree is not more than 1.33 multiplied by 10-1Pa) degassing the titanium chips;
2) treating parts before entering the furnace: according to a part cleaning program, manually cleaning the part by using acetone or an alcohol solvent, and cleaning the part before furnace installation by combining an alkali cleaning (Isoprep 44# cleaning agent) mode if necessary, wherein a water film on the surface of the part is ensured to be continuous in the water washing process of the alkali cleaning, and finally wiping the part dry or drying the part dry by using clean compressed air;
3) vacuum heat treatment process: loading the parts on the cleaned tool in the step 1), preventing nesting, stacking or matching, placing the parts in a manner of a layer of titanium chips and a layer of parts, laying a layer of titanium chips on the outermost layer of parts, and heating the parts in an effective working area; setting technological parameters, controlling the vacuum degree in the furnace to be less than or equal to 1.33 multiplied by 10 < -1 > Pa, heating to 482 +/-14 ℃, preserving the temperature for at least 1 hour, refilling high-purity argon gas after preserving the temperature until the temperature in the furnace is cooled to be less than or equal to 371 ℃, stopping refilling the argon gas, continuing cooling in the furnace, opening the door when the temperature reaches below 200 ℃, taking out the part, and cooling in air; wherein, the thickness of the parts in the furnace is less than or equal to 25mm, and when the thickness of the parts is increased by 25mm, the heat preservation time is prolonged by 1 hour;
4) and (3) inspection and packaging transfer: after the parts are taken out of the furnace, the parts are taken, placed and inspected by wearing clean white gloves, and the parts are packaged by polyethylene bags or kraft paper bags and then transferred to the next procedure.
The precipitation hardening stainless steel joint part after heat treatment by the method has uniform film layer after surface passivation and has no iridescence such as yellow, blue and the like.
Claims (2)
1. A method for preventing stainless steel from being oxidized by heat treatment is characterized by comprising the following steps:
1) preparing a tool, titanium chips and the like: manually cleaning the tool and the fixture by using acetone or alcohol, and drying; collecting titanium scraps Ti-6Al-4V, soaking and cleaning with acetone, then carrying out alkali cleaning, finally washing with water and drying; before each production, degassing titanium chips at a temperature not lower than the heating temperature of the part and under a vacuum degree in advance;
2) treating parts before entering the furnace: according to a part cleaning program, manually cleaning the part by using acetone or alcohol solvent, and cleaning the part before furnace installation by combining an alkali cleaning mode if necessary, wherein a water film on the surface of the part is ensured to be continuous in an alkali cleaning water washing process, and finally wiping the part dry or drying the part by using clean compressed air;
3) vacuum heat treatment process: loading the parts on the cleaned tool in the step 1), preventing nesting, stacking or matching, placing the parts in a manner of a layer of titanium chips and a layer of parts, laying a layer of titanium chips on the outermost layer of parts, and heating the parts in an effective working area; setting technological parameters, controlling the vacuum degree in the furnace to be less than or equal to 1.33 multiplied by 10-1Pa, heating to 482 +/-14 ℃, preserving heat for at least 1 hour, refilling high-purity argon until the temperature in the furnace is cooled to be less than or equal to 371 ℃, stopping refilling argon, continuing cooling the part in the furnace, opening the door when the temperature reaches below 200 ℃, taking out the part, and air-cooling;
4) and (3) inspection and packaging transfer: after the parts are taken out of the furnace, the parts are taken, placed and inspected by wearing clean white gloves, and the parts are packaged by polyethylene bags or kraft paper bags and then transferred to the next procedure.
2. The method for preventing oxidation in a heat treatment of stainless steel according to claim 1, wherein: the thickness of the part in the step 3) is less than or equal to 25mm, and when the thickness of the part is increased by 25mm, the heat preservation time is prolonged by 1 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911250224.7A CN110835673A (en) | 2019-12-09 | 2019-12-09 | Method for preventing stainless steel from being oxidized during heat treatment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911250224.7A CN110835673A (en) | 2019-12-09 | 2019-12-09 | Method for preventing stainless steel from being oxidized during heat treatment |
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| CN110835673A true CN110835673A (en) | 2020-02-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115464008A (en) * | 2022-08-30 | 2022-12-13 | 北京航空材料研究院股份有限公司 | Method and tool for calibrating titanium alloy rear base |
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| CN1376210A (en) * | 1999-07-28 | 2002-10-23 | 安东尼诺·乔治·卡卡切 | Process for manufacturing corrosion resistant metal products |
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| EP3176277A1 (en) * | 2014-07-29 | 2017-06-07 | Nippon Steel & Sumikin Stainless Steel Corporation | Ferritic stainless steel material for fuel cell, and method for producing same |
| CN107974653A (en) * | 2017-12-01 | 2018-05-01 | 中国航空工业标准件制造有限责任公司 | A kind of underproof optimization method of titanium-niobium alloy part annealing heat-treats |
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| JP2019183193A (en) * | 2018-04-03 | 2019-10-24 | 日本製鉄株式会社 | Austenite stainless steel |
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2019
- 2019-12-09 CN CN201911250224.7A patent/CN110835673A/en active Pending
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| CN101423922A (en) * | 2007-11-02 | 2009-05-06 | 中国船舶重工集团公司第七二五研究所 | Heat treating process of titanium alloy in antivacuum furnace |
| EP3176277A1 (en) * | 2014-07-29 | 2017-06-07 | Nippon Steel & Sumikin Stainless Steel Corporation | Ferritic stainless steel material for fuel cell, and method for producing same |
| CN107974653A (en) * | 2017-12-01 | 2018-05-01 | 中国航空工业标准件制造有限责任公司 | A kind of underproof optimization method of titanium-niobium alloy part annealing heat-treats |
| JP2019183193A (en) * | 2018-04-03 | 2019-10-24 | 日本製鉄株式会社 | Austenite stainless steel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115464008A (en) * | 2022-08-30 | 2022-12-13 | 北京航空材料研究院股份有限公司 | Method and tool for calibrating titanium alloy rear base |
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Application publication date: 20200225 |
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