CN103088283B - Sectional type pressurizing solid solution nitriding accelerating method of austenitic stainless steel - Google Patents
Sectional type pressurizing solid solution nitriding accelerating method of austenitic stainless steel Download PDFInfo
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- 238000005121 nitriding Methods 0.000 title claims abstract description 65
- 239000006104 solid solution Substances 0.000 title claims abstract description 45
- 229910000963 austenitic stainless steel Inorganic materials 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 6
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 125000004433 nitrogen atom Chemical group N* 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910001039 duplex stainless steel Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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Abstract
一种奥氏体不锈钢分段式加压固溶氮化催渗方法,其主要是:将奥氏体不锈钢置于专利名称为“一种具有双压平衡结构的增压高温氮化装置”专利号为201210530358.6固溶氮化炉中,并以0.5-2L/min流速通入NH3至炉内压强到达0.1~1.0MPa范围,在温度为500~700℃下进行NH3氮化预处理5~10h;再将上述固溶氮化炉内NH3完全排出并以1-5L/min流速通入N2至炉内压强到达0.1~1.0MPa范围,后将炉温迅速升至900~1200℃,在此条件下进行N2固溶氮化处理1~20h,随后快速水冷至室温,在奥氏体不锈钢表面形成固溶氮化层。本发明可提高氮化效率,增加渗层的整体氮含量,有效减缓甚至避免氮化过程中渗件晶粒粗化。A stepwise pressurized solid solution nitriding and catalytic infiltration method for austenitic stainless steel, which mainly includes: placing austenitic stainless steel in the patent titled "a pressurized high-temperature nitriding device with a double-pressure balance structure" No. 201210530358.6 solid solution nitriding furnace, and NH 3 is passed into the furnace at a flow rate of 0.5-2L/min until the pressure in the furnace reaches the range of 0.1-1.0MPa, and NH 3 nitriding pretreatment is carried out at a temperature of 500-700°C for 5- 10h; then completely discharge the NH 3 in the above-mentioned solid solution nitriding furnace and feed N 2 at a flow rate of 1-5L/min until the pressure in the furnace reaches the range of 0.1-1.0MPa, and then rapidly raise the furnace temperature to 900-1200°C, Under these conditions, N2 solid solution nitriding treatment is carried out for 1 to 20 hours, followed by rapid water cooling to room temperature to form a solid solution nitriding layer on the surface of austenitic stainless steel. The invention can improve the nitriding efficiency, increase the overall nitrogen content of the nitriding layer, and effectively slow down or even avoid the grain coarsening of the nitriding part during the nitriding process.
Description
技术领域technical field
本发明涉及一种金属表面化学热处理方法,特别是奥氏体不锈钢的固溶氮化方法。The invention relates to a metal surface chemical heat treatment method, in particular to a solid solution nitriding method for austenitic stainless steel.
背景技术Background technique
作为一种新型表面化学热处理技术,固溶氮化已广泛应用于医药、化工、机械制造等生产中。传统的固溶氮化一般是在高温(1050~1200℃)和一定压力的氮气气氛中实现的。为增加固溶氮化层厚度及氮含量,需在高温N2环境中进行长时间的保温处理,以保证N2大量分解出活性N原子并获得较高的扩散速度,这就不可避免地导致奥氏体不锈钢的晶粒粗化和整体性能恶化,并加大工业生产中设备的损耗速度。因此,固溶氮化周期的长短将直接影响渗件的整体质量。As a new surface chemical heat treatment technology, solid solution nitriding has been widely used in the production of medicine, chemical industry, machinery manufacturing and so on. Traditional solid solution nitriding is generally realized at high temperature (1050-1200°C) and a certain pressure of nitrogen atmosphere. In order to increase the thickness and nitrogen content of the solid solution nitriding layer, it is necessary to carry out a long-term heat preservation treatment in a high-temperature N2 environment to ensure that N2 decomposes a large amount of active N atoms and obtains a higher diffusion rate, which inevitably leads to The grain coarsening and overall performance deterioration of austenitic stainless steel will increase the wear rate of equipment in industrial production. Therefore, the length of the solid solution nitriding cycle will directly affect the overall quality of the parts.
通过对现有技术的检索,发现由作者Fu Rui-dong发表一文“Solid SolutionNitriding Technology of 15Cr-7.5Mn-2.6Mo Duplex Stainless Steel”中采用了高温多段固溶氮化,但其各段工艺的温度均大于1050℃,并未从根本上降低固溶氮化温度。文献《奥氏体不锈钢的氨气渗氮处理》中采用三段式氮化工艺,三段温度不同,但氮化介质均为NH3,N原子未固溶于不锈钢表层,有氮化物析出。Through the retrieval of the prior art, it was found that the article "Solid Solution Nitriding Technology of 15Cr-7.5Mn-2.6Mo Duplex Stainless Steel" published by the author Fu Rui-dong used high-temperature multi-stage solid solution nitriding, but the temperature of each stage of the process Both are greater than 1050°C, and the solid solution nitriding temperature has not been fundamentally reduced. In the document "Ammonia Nitriding Treatment of Austenitic Stainless Steel", a three-stage nitriding process is adopted. The temperature of the three stages is different, but the nitriding medium is NH 3 , and the N atoms are not solid-dissolved in the surface of the stainless steel, and nitrides are precipitated.
发明内容Contents of the invention
本发明的目的在于提供一种可提高氮化效率,增加渗层的整体氮含量,有效减缓甚至避免氮化过程中渗件晶粒粗化的奥氏体不锈钢分段式加压固溶氮化催渗方法。本发明主要是:采用不同介质依次在低温和高温两段区间进行氮化处理,随后快速水冷至室温,在奥氏体不锈钢表面形成固溶氮化层。The object of the present invention is to provide a segmental pressurized solid solution nitriding of austenitic stainless steel which can improve the nitriding efficiency, increase the overall nitrogen content of the permeated layer, and effectively slow down or even avoid the grain coarsening of the permeated parts during the nitriding process. Infiltration method. The present invention mainly comprises: using different media to sequentially carry out nitriding treatment in two sections of low temperature and high temperature, and then quickly water cooling to room temperature to form a solid solution nitriding layer on the surface of the austenitic stainless steel.
本发明的技术方案如下:Technical scheme of the present invention is as follows:
(1)将奥氏体不锈钢置于专利名称为“一种具有双压平衡结构的增压高温氮化装置”、申请号为201210530358.6的固溶氮化炉中,并以0.5-2L/min流速通入NH3至炉内压强到达氮化压强0.1~1.0MPa范围,在温度为500~700℃下进行NH3氮化预处理5~10h。(1) Place the austenitic stainless steel in the solid solution nitriding furnace with the patent name "A pressurized high-temperature nitriding device with dual-pressure balance structure" and the application number 201210530358.6, and flow at a flow rate of 0.5-2L/min Introduce NH 3 until the pressure in the furnace reaches the nitriding pressure range of 0.1-1.0 MPa, and carry out NH 3 nitriding pretreatment at a temperature of 500-700°C for 5-10 hours.
(2)将上述申请号为201210530358.6的固溶氮化炉内NH3完全排出并通入N2至炉内压强到达0.1~1.0MPa范围,该N2流量为1-5L/min,后将炉温迅速升至900~1200℃进行N2固溶氮化处理1~20h,随后快速水冷至室温,在奥氏体不锈钢表面形成固溶氮化层。(2) Completely discharge the NH3 in the solid solution nitriding furnace with the above application number 201210530358.6 and feed N2 until the pressure in the furnace reaches the range of 0.1-1.0MPa. The N2 flow rate is 1-5L/min, and then the furnace The temperature is rapidly raised to 900-1200°C for N 2 solid solution nitriding treatment for 1-20 hours, and then rapidly cooled to room temperature with water to form a solid solution nitriding layer on the surface of austenitic stainless steel.
本发明与现有技术相比具有如下优点:Compared with the prior art, the present invention has the following advantages:
1、在整个氮化过程中都具备相对较高的渗速,低温高速强渗在于NH3在较低(500~700℃)温度便分解出活性N原子,通过加压和增加流量获得高氮势,在奥氏体不锈钢表面先制备出表层富氮区或使其表面产生较高的N浓度梯度,藉此保证在高温氮化阶段有效促进N原子的扩散,提高N含量及渗层厚度。1. It has a relatively high permeation rate throughout the nitriding process. The low-temperature and high-speed strong permeation is due to the fact that NH3 decomposes into active N atoms at a relatively low temperature (500-700°C), and high nitrogen is obtained by pressurizing and increasing the flow rate. Potential, on the surface of austenitic stainless steel, first prepare the surface nitrogen-rich area or make the surface produce a higher N concentration gradient, so as to ensure that the diffusion of N atoms can be effectively promoted in the high-temperature nitriding stage, and the N content and the thickness of the infiltrated layer can be increased.
2、利用此分段式工艺对奥氏体不锈钢固溶氮化处理得到的渗层厚度大于两段工艺分离实施所得氮化层深度的叠加,加速氮化效果显著,不但获得了更高的N含量和硬度,而且大大提高了固溶氮化效率,明显减小渗件的晶粒长大倾向。2. Using this staged process to treat austenitic stainless steel with solid solution nitriding treatment, the thickness of the infiltrated layer is greater than the superimposition of the depth of the nitrided layer obtained by the separation of the two stages of technology. The accelerated nitriding effect is remarkable, and not only a higher N content and hardness, and greatly improve the efficiency of solid solution nitriding, significantly reducing the tendency of grain growth of infiltrated parts.
3、在同样的氮含量及渗层厚度要求下,采用该工艺可以有效缩短高温段氮化时间(或降低氮化温度),提高固溶氮化效率,缩短固溶氮化工艺周期,降低成本及设备损耗。3. Under the same nitrogen content and thickness requirements of the infiltrated layer, this process can effectively shorten the nitriding time in the high temperature section (or reduce the nitriding temperature), improve the efficiency of solid solution nitriding, shorten the process cycle of solid solution nitriding, and reduce costs and equipment loss.
附图说明Description of drawings
图1是本发明实施例1获得的固溶氮化层微观组织图。Figure 1 is a microstructure diagram of the solid solution nitrided layer obtained in Example 1 of the present invention.
图2是本发明实施例2获得的固溶氮化层微观组织图。Fig. 2 is a microstructure diagram of the solid solution nitrided layer obtained in Example 2 of the present invention.
图3是本发明实施例3获得的固溶氮化层微观组织图。Fig. 3 is a microstructure diagram of a solid solution nitrided layer obtained in Example 3 of the present invention.
具体实方式:The specific way:
实施例1:Example 1:
将304奥氏体不锈钢加工成薄板悬挂于专利名称为“一种具有双压平衡结构的增压高温氮化装置”、申请号为201210530358.6的固溶氮化炉中,并以0.5L/min通入NH3气,升温至500℃,在0.25MPa加压条件下氮化10h。然后将上述申请号为201210530358.6的固溶氮化炉内NH3排出并以流量为5L/min通入N2,迅速升温至1150℃,在0.25MPa加压条件下固溶氮化10h,而后迅速水冷至室温。本实施例所得固溶氮化层厚度可达311μm左右,如图1所示。Process 304 austenitic stainless steel into a thin plate and hang it in a solid solution nitriding furnace with the patent name "A pressurized high-temperature nitriding device with a double-pressure balance structure" and application number 201210530358.6, and pass it at 0.5L/min Inject NH 3 gas, raise the temperature to 500°C, and nitriding for 10h under the pressure condition of 0.25MPa. Then discharge the NH 3 in the solid solution nitriding furnace with the above application number 201210530358.6 and feed N 2 at a flow rate of 5L/min, rapidly raise the temperature to 1150°C, and perform solid solution nitriding under 0.25MPa pressure for 10 hours, and then quickly Water cooled to room temperature. The solid solution nitrided layer obtained in this example has a thickness of about 311 μm, as shown in FIG. 1 .
实施例2:Example 2:
将304奥氏体不锈钢加工成薄板悬挂于专利名称为“一种具有双压平衡结构的增压高温氮化装置”专利号为201210530358.6固溶氮化炉中,并以1L/min通入NH3气,升温至700℃,在0.1MPa加压条件下氮化5h。然后将上述申请号为201210530358.6的固溶氮化炉内NH3排出并以流量为3L/min通入N2,迅速升温至1050℃,在0.15MPa加压条件下固溶氮化10h,而后迅速水冷至室温。本实施例所得固溶氮化层厚度可达160μm左右,如图2所示。Process 304 austenitic stainless steel into a thin plate and hang it in the solid solution nitriding furnace with the patent name "A pressurized high-temperature nitriding device with a double-pressure balance structure" patent number 201210530358.6, and feed NH 3 at 1L/min gas, heated to 700°C, and nitrided for 5h under the pressure of 0.1MPa. Then discharge the NH 3 in the solid solution nitriding furnace with the above application number 201210530358.6 and feed N 2 at a flow rate of 3L/min, rapidly raise the temperature to 1050°C, and perform solid solution nitriding under 0.15MPa pressure for 10 hours, and then quickly Water cooled to room temperature. The solid solution nitrided layer obtained in this embodiment has a thickness of about 160 μm, as shown in FIG. 2 .
实施例3:Example 3:
将316奥氏体不锈钢加工成薄板悬挂于专利名称为“一种具有双压平衡结构的增压高温氮化装置”专利号为201210530358.6固溶氮化炉中,并以1L/min通入NH3气,升温至600℃,在1.0MPa加压条件下氮化5h。然后将上述申请号为201210530358.6的固溶氮化炉内NH3排出并以流量为5L/min通入N2,迅速升温至900℃,在1.0MPa加压条件下固溶氮化1h,而后迅速水冷至室温。本实施例所得固溶氮化层厚度可达90μm左右,如图3所示。Process 316 austenitic stainless steel into a thin plate and hang it in the solid solution nitriding furnace with the patent name "A pressurized high-temperature nitriding device with a double-pressure balance structure" patent number 201210530358.6, and feed NH 3 at 1L/min gas, the temperature was raised to 600°C, and nitriding was carried out for 5 hours under the pressure of 1.0MPa. Then discharge the NH 3 in the solid-solution nitriding furnace with the above application number 201210530358.6 and feed N 2 at a flow rate of 5L/min, rapidly raise the temperature to 900°C, perform solid-solution nitriding under 1.0MPa pressure for 1 hour, and then quickly Water cooled to room temperature. The solid solution nitrided layer obtained in this embodiment has a thickness of about 90 μm, as shown in FIG. 3 .
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