CN102560507A - Surface treatment method for nitrided case of steel material - Google Patents
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Abstract
The invention belongs to the technical field of material processing, and particularly relates to a surface treatment method for a nitrided case of a steel material. The invention adopts the technical scheme that the method comprises the steps of performing nitriding treatment on nitrided steel which is then loaded into an ion nitriding furnace, starting a vacuum pump in which 200-600Pa hydrogen or argon is charged, starting 500-700V voltage, ionizing gases with high voltage, heating a sample to 500-650 DEG C, performing ion bombardment on a decomposed chemical compound layer on the surface of the steel, carrying out surface nanocrystallization on the steel product sample after the ion bombardment, and then obtaining a pure diffusion layer structure on the surface of the steel product sample; the surface layer of the pure diffusion layer structure is in nano dimension; the hardness of the pure diffusion layer structure is more than or equal to 1240HV; and the nitriding brittleness is Class 1. In the method, the ion bombardment method is used to decompose the chemical compound layer after the nitriding treatment to eliminate the brittleness, then the surface of the steel product is subjected to the surface nanocrystallization to improve the hardness and the abrasive resistance of the sample, and finally the surface layer with high strength and high toughness is obtained; the method has the advantages that the operation is simple, the equipment is mature, the cost is lower, and the production efficiency is higher.
Description
Technical field
The invention belongs to the materials processing technology field, be specifically related to a kind of surface treatment method of ferrous materials nitrided case.
Background technology
In industrial circle, surface carburization is handled and usually is used for improving surface hardness, wear resistance and fatigue strength of ferrous materials or the like.Nitridation process has remarkable advantages aspect surface strengthening technology, be widely used in power machine-building industry, as the bent axle in the axle sleeve of steam turbine and all kinds of valve, valve rod, the oil motor, steam jacket, fuel distributing pump component, plunger to needle valve etc.Its technological process is exactly to make nitrogen-atoms infiltrate the chemical heat treatment method of workpiece surface in a kind of certain at a certain temperature medium, and common nitriding method has liquid nitriding, gas nitriding and ionitriding.In nitriding process, nitrogen-atoms can spread to material internal along material crystal boundary and other defect, when the top layer nitrogen atom concentration acquires a certain degree, will form ε-Fe
3-2N and γ '-Fe
4Nitride such as N, these nitride are commonly called as " compound layer " or " bright layer " from the nitride layer that single nucleus begins to form rapidly a sealing.Compound layer has very high hardness; Good wear resistance and solidity to corrosion, however they but have very big fragility, and the bright layer of therefore being made up of these nitride breaks under stress condition easily; Broken hard material can sharply damage the mating material both sides; Wear particle even can be attached on causes the secondary injury on other part, and the crack tip when breaking can convert the fatigue cracking source into very soon, reduces the fatigue lifetime of workpiece.That is to say the existence of bright layer; Cause mechanical accident easily and have a strong impact on the work-ing life of workpiece under some a particular job environment; In the nitriding strength member (introducing FSU's technology) of the fifties aircraft industry in last century, clearly regulation is just arranged, the nitriding piece surface does not allow bright layer and exists.Therefore nitrided case toughness how to improve steel is the problem that people comparatively pay close attention to, and early stage terms of settlement is to remove bright layer with the way of grinding, only keeps more tough diffusion layer, but because the difficulty in the processing, difficult technique causes scrap rate higher with control.Under appointed condition at that time, from nitridation process control, thought also that quite a lot of methods all not have successfully, people had specialized in a kind of extraordinary etching reagent and had removed bright layer afterwards, though see effect, undesirable, hypertoxic in addition, have to abandon.
The industrial at present method that goes up nitrogen content in control nitriding process commonly used removes to obtain the nitrided case of H.T., and its method is in whole nitriding process, keeps lower nitrogen concentration, to avoid generation γ '-Fe on the surface
4The nucleus of N or other nitride; The nitrogen gesture of this moment only is lower than formation nitride threshold value just, so that diffusion layer can be saturated by nitrogen institute, but the drawback that this method is brought is the top layer performance of steel; Like the decline of hardness and wear resistance, process cycle is grown and is wasted energy.In addition, the method for ion bombardment is also comparatively commonly used, and its principle is that the workpiece after the traditional technology nitriding is packed in the ionitriding equipment; With hydrogen or argon gas is medium, leans on the photoglow ionized gas, and the gas bombardment sample surfaces after the ionization decomposes established compound layer; Though this method has also solved the fragility problem of nitrided case effectively; But equally also can bring some negative impacts, like the hardness reduction of nitrided case, all more traditional nitridation process of solidity to corrosion and wear resistance reduces a lot of.Therefore how to prepare HS, the nitrided case of H.T. is the difficult problem that present steel material surface is handled.
Literature search to existing technology is found; W.P.Tong etc. are in " Science " (" science "; 2003 299 volume 686-688 pages or leaves) delivered the paper that is entitled as " Nitriding Iron at Lower Temperatures " (" the low temperature nitriding of iron "); Discovery utilizes the making Nano surface technology can reduce traditional nitriding temperature greatly, but this making Nano surface low temperature nitridation technique does not solve the fragility problem of nitrided case.
Summary of the invention
To the weak point of the brittle method of present solution ferrous materials nitrided case, the present invention provides a kind of surface treatment method of ferrous materials nitrided case, adopts ion bombardment and making Nano surface process combined to prepare and has HS and H.T. nitrided case.
The technical scheme of realization the object of the invention is carried out according to following steps:
(1) choosing nitriding steel is raw material, adopts the method for ionitriding that steel are carried out nitriding treatment, and the steel textura epidermoidea after the nitrogenize is for comprising ε-Fe
3-2N and γ '-Fe
4The compound layer of N and the diffusion layer that comprises α-Fe, surface hardness is 1000-1200HV;
(2) will the steel after nitriding is handled after ultrasonic cleaning, pack in the ion nitriding furnace, start vacuum pump, ion-nitriding furnace is evacuated to 0.4-1Pa; Open hydrogen or argon gas that gas meter charges into 200-600Pa then; Start the voltage of 500-700V, utilize high-voltage to be heated to 500-650 ℃, ion bombardment steel surface decomposition compound layer with ionization of gas and with sample; Insulation 4-12h; In 3-5 minute, gas flow is reduced to zero then, remove voltage, steel sample naturally cools to room temperature;
The steel sample that (3) will pass through ion bombardment in the making Nano surface trier of packing into, carries out Surface Nanocrystalline to steel surface after ultrasonic cleaning; With diameter is the bottom that the Cr15 steel ball of 3-8mm is placed on the sample chamber; Steel ball is 28-40mm apart from the steel sample surface, and the ultrasonic vibration frequency that the head that shakes is set is 20KHz, drives steel ball through ultrasonic vibration the steel sample surface is clashed into; Treatment time is 2-4h; Obtaining the top layer on the steel sample surface at last is the pure diffusion layer tissue of nano-scale, its hardness >=1240HV, and nitriding fragility is 1 grade.
Described nitriding steel comprises 20CrMo steel and 38CrMoAl steel, but is not limited only to above-mentioned two kinds, also comprises industrial all common nitriding steels at present.
Wherein the present invention is not limited only to ionitriding to the method that steel carry out nitriding treatment, in the prior art steel is carried out the technology that nitriding handles and all is applicable to this step.
Principle of the present invention is at first to utilize the method for ion bombardment to decompose the compound layer after nitriding is handled; To eliminate its fragility; But the negative impact that such method is brought is exactly the decline that makes its hardness and wear resistance; So we continue Surface Nanocrystalline has been carried out on the surface of sample, to promote the hardness and the wear resistance of sample, final comprehensive two kinds of methods obtain the steel nitriding top layer of high-intensity high-tenacity.
The invention has the beneficial effects as follows and improved the nitrided case fragility problem that traditional nitridation process exists effectively, and improved the hardness and the wear resistance on steel nitriding top layer to a certain extent, still do not have additive method at present and accomplish; Be in same ion-nitriding furnace, to carry out with the ion bombardment step after the ionitriding step of the present invention, only need to regulate atmosphere, pressure and other parameters, simple to operate, equipment is ripe, and cost is lower, and production efficiency is higher.
Description of drawings
Fig. 1 is the X-ray diffractogram of the sample of the embodiment of the invention 3 preparations;
Fig. 2 is the microhardness of the sample of the embodiment of the invention 3 preparations;
Fig. 3 is the sample top layer and the prepared sample surface brittleness comparison diagram of traditional nitridation process of the embodiment of the invention 3 preparations.
Embodiment
The employed device of the embodiment of the invention is LOCMT-15A ion-nitriding furnace and SNC-2 type making Nano surface experimental machine,
The embodiment of the invention adopts PW3040/60 X ' Pert Pro type X diffractometer that sample top layer phase structure is analyzed; With L101MVD digital display micro Vickers specimen transverse section hardness and surface brittleness, with the wear resistance on the reciprocal experimental machine specimen of Optimol SRV type ball disc type top layer.
Below in conjunction with concrete embodiment technical scheme of the present invention and technique effect are further specified.
Embodiment 1
With the 20CrMo steel is starting material, and sample is packed in the ion-nitriding furnace at 500 ℃ of nitriding 4h, finds to obtain the thick compound layer of 15 μ m on the sample top layer through metaloscope and x-ray analysis, and compound layer comprises ε-Fe
3-2N and γ '-Fe
4Two kinds of nitride of N; Steel sample surface hardness after the nitriding is 1080HV, has sizable fragility through the microhardness tester specimen, is decided to be three grades of fragility.
In the ion-nitriding furnace of packing into after the 20CrMo steel sample ultrasonic cleaning after the nitriding processing, be evacuated to 0.4Pa, feed the argon gas of 200Pa; Making alive adopts the method for high-voltage glow-discharge that sample is heated to 500 ℃ to 500V, insulation 4h; High pressure utilizes ion bombardment that compound layer is decomposed ionization of gas, and insulation finishes in back 3 minutes; With voltage and gas flow modulation is zero, and the steel sample air cooling is to room temperature; Steel sample to after the ion bombardment processing can know that through X-ray analysis the sample top layer has only α-Fe phase basically, and through the microhardness tester test, the hardness on sample top layer is 700HV and has lower fragility, is decided to be 1 grade of fragility.
Steel sample after will passing through ion bombardment and the handling making Nano surface trier of packing into; The diameter of packing in the bottom, sample chamber is the Cr15 steel ball of 3mm, and steel ball is made as 30mm from the distance of steel sample, and a frequency of shaking is made as 20KHz; Treatment time is 2h, obtains final steel sample; Through the microhardness tester test, its surface hardness reaches 1250HV, and the wear resistance experiment shows that wear resistance is good, and impression test shows that surface brittleness is good, does not have obvious crackle around the impression, is decided to be 1 grade of fragility.
Embodiment 2
With the 20CrMo steel is starting material, and sample is packed in the ion-nitriding furnace in 530 ℃ of nitriding 5h, finds to obtain the thick compound layer of 19 μ m on the top layer through metaloscope and x-ray analysis, and compound layer comprises ε-Fe
3-2N and γ '-Fe
4N two phases; The surface hardness of sample is 1130HV after the nitriding, has sizable fragility through the microhardness tester specimen, is decided to be 3 grades of fragility.
In the ion-nitriding furnace of packing into after the 20CrMo steel sample ultrasonic cleaning after the nitriding processing, be evacuated to 1Pa, feed the argon gas of 330Pa; Making alive adopts high-voltage glow-discharge that sample is heated to 600 ℃ to 600V, insulation 8h; High pressure utilizes the method for ion bombardment that compound layer is decomposed ionization of gas, and insulation finishes in back 3 minutes; Voltage and gas flow are reduced to zero, and the sample air cooling is to room temperature.Can know that through X-ray analysis the sample top layer has only α-Fe phase basically, through the microhardness tester test, the hardness on sample top layer is 660HV, and has lower fragility.
The sample that will the pass through ion bombardment face nanometer trier of packing into, the diameter of packing in the bottom, sample chamber is the Cr15 steel ball of 4mm, and steel ball is made as 28mm from the distance of sample, and a frequency of shaking is made as 20KHz, and the treatment time is 3h, obtains final sample; Find that through the microhardness tester test surface hardness of steel sample reaches 1250HV, surface brittleness is good, does not have obvious crackle around the impression, be decided to be 1 grade of fragility, and wear-resisting experiment shows that the sample wear resistance is good.
Embodiment 3
With the 20CrMo steel is starting material, and sample is packed in the ion-nitriding furnace in 530 ℃ of nitriding 5h, finds to obtain the thick compound layer of 19 μ m on the steel sample top layer through metaloscope and x-ray analysis, and compound layer comprises ε-Fe
3-2N and γ '-Fe
4N two phases; The surface hardness of steel sample is 1130HV after the nitriding, has sizable fragility through the microhardness tester specimen, is decided to be 3 grades of fragility.
In the ion-nitriding furnace of packing into after the 20CrMo steel ultrasonic cleaning after the nitriding processing, be evacuated to 0.5Pa, feed the hydrogen of 500Pa; Making alive adopts high-voltage glow-discharge that sample is heated to 600 ℃ to 600V, insulation 10h; High pressure is with ionization of gas; Utilize ion bombardment that compound layer is decomposed, insulation finishes in back 3 minutes voltage and gas flow to be reduced to zero, and the steel sample air cooling is to room temperature; Can know that through X-ray analysis the sample top layer has only α-Fe phase basically, through the microhardness tester test, the hardness on sample top layer is 755HV, and has lower fragility, is decided to be 1 grade of fragility.
The steel sample that will the pass through ion bombardment making Nano surface trier of packing into, the diameter of packing in the bottom, sample chamber is the Cr15 steel ball of 6mm, and steel ball is made as 28mm from the distance of sample, and a frequency of shaking is made as 20KHz, and the treatment time is 3h, obtains final steel sample; Find that through the microhardness tester test surface hardness of steel sample reaches 1340HV, as shown in Figure 2; The impression test that Fig. 3 (b) and 3 (d) are shown shows that the sample surface brittleness is good, do not have obvious crackle around the impression, and wear-resisting experiment shows that the sample wear resistance is good.
Embodiment 4
With the 20CrMo steel is starting material, with the sample 530 ℃ of nitriding 5h in the ion-nitriding furnace that pack into, finds that through metaloscope and x-ray analysis obtain the compound layer of 19 μ m on the steel sample top layer, compound layer comprises ε-Fe
3-2N and γ '-Fe
4N two phases; The surface hardness of the steel sample after the nitriding is 1130HV, has sizable fragility through the microhardness tester specimen, is decided to be 3 grades of fragility.
In the ion-nitriding furnace of packing into after the 20CrMo steel ultrasonic cleaning after the nitriding processing, be evacuated to 0.8Pa, feed the argon gas of 600Pa; Making alive adopts high-voltage glow-discharge that sample is heated to 630 ℃ to 650V, insulation 10h; High pressure is with ionization of gas; Utilize ion bombardment that compound layer is decomposed, insulation finishes in back 4 minutes voltage and gas flow to be reduced to zero, and the steel sample air cooling is to room temperature; Can know that through X-ray analysis the steel sample top layer has only α-Fe phase basically, through the microhardness tester test, the hardness on sample top layer is approximately 710HV and has lower fragility, is decided to be 1 grade of fragility.
The sample that will the pass through ion bombardment making Nano surface trier of packing into, the diameter of packing in the bottom, sample chamber is the Cr15 steel ball of 6mm, and steel ball is made as 35mm from the distance of sample, and a frequency of shaking is made as 20KHz, and the treatment time is 3h, obtains final steel sample; Find that through the microhardness tester test surface hardness reaches 1320HV, surface brittleness is good, does not have obvious crackle around the impression, is decided to be 1 grade of fragility, and wear-resisting experiment shows that the sample wear resistance is good.
Embodiment 5
With the 38CrMoAl steel is starting material, with the sample 530 ℃ of nitriding 3h in the ion-nitriding furnace that pack into, and through metaloscope and x-ray analysis, the compound layer after the steel top layer obtains 13 μ m, compound layer mainly comprises ε-Fe
3-2N and γ '-Fe
4N two phases; The surface hardness of the steel sample after the nitriding is 1180HV, has sizable fragility through the microhardness tester specimen, is decided to be 4 grades of fragility.
After the 38CrMoAl steel sample ultrasonic cleaning after the nitriding processing, in the ion-nitriding furnace of packing into, be evacuated to 0.5Pa; Feed the argon gas of 300Pa, making alive adopts high-voltage glow-discharge that sample is heated to 630 ℃ to 650V; Insulation 12h, high pressure utilizes ion bombardment that compound layer is decomposed ionization of gas; Insulation finishes in back 5 minutes voltage and gas flow to be reduced to zero, and the steel sample air cooling is to room temperature; Can know that through X-ray analysis the sample top layer has only α-Fe phase basically, through the microhardness tester test, the hardness on sample top layer is 720HV and has lower fragility, is decided to be 1 grade of fragility.
The sample that will the pass through ion bombardment making Nano surface trier of packing into, the Cr15 steel ball of the diameter 4mm that packs in the bottom, sample chamber, steel ball is made as 35mm from the distance of sample, and a frequency of shaking is made as 20KHz, and the treatment time is 3h, obtains final sample; Find that through microhardness tester tests the steel sample surface hardness reaches 1240HV, surface brittleness is good, does not have obvious crackle around the impression, and wear-resisting experiment shows that the sample wear resistance is good, is decided to be 1 grade of fragility.
Embodiment 6
With the 38CrMoAl steel is starting material, with the sample 530 ℃ of nitriding 3h in the ion-nitriding furnace that pack into, and through metaloscope and x-ray analysis, the compound layer after the steel top layer obtains 13 μ m, compound layer mainly comprises ε-Fe
3-2N and γ '-Fe
4N two phases; The surface hardness of the steel sample after the nitriding is 1180HV, has sizable fragility through the microhardness tester specimen, is decided to be 4 grades of fragility.
After the 38CrMoAl steel sample ultrasonic cleaning after the nitriding processing, in the ion-nitriding furnace of packing into, be evacuated to 0.5Pa; Feed the argon gas of 300Pa, making alive adopts high-voltage glow-discharge that sample is heated to 650 ℃ to 700V; Insulation 12h, high pressure utilizes ion bombardment that compound layer is decomposed ionization of gas; Insulation finishes in back 5 minutes voltage and gas flow to be reduced to zero, and the steel sample air cooling is to room temperature; Can know that through X-ray analysis the sample top layer has only α-Fe phase basically, through the microhardness tester test, the hardness on sample top layer is 720HV and has lower fragility, is decided to be 1 grade of fragility.
The sample that will the pass through ion bombardment making Nano surface trier of packing into, the Cr15 steel ball of the diameter 8mm that packs in the bottom, sample chamber, steel ball is made as 40mm from the distance of sample, and a frequency of shaking is made as 20KHz, and the treatment time is 3h, obtains final sample; Find that through microhardness tester tests the steel sample surface hardness reaches 1240HV, surface brittleness is good, does not have obvious crackle around the impression, and wear-resisting experiment shows that the sample wear resistance is good, is decided to be 1 grade of fragility.
Claims (2)
1. the surface treatment method of a ferrous materials nitrided case is characterized in that carrying out according to following steps:
(1) choosing nitriding steel is raw material, adopts the method for ionitriding that steel are carried out nitriding treatment, and the steel textura epidermoidea after the nitrogenize is for comprising ε-Fe
3-2N and γ '-Fe
4The compound layer of N and the diffusion layer that comprises α-Fe, surface hardness is 1000-1200HV;
(2) will the steel after nitriding is handled after ultrasonic cleaning, pack in the ion nitriding furnace, start vacuum pump, ion-nitriding furnace is evacuated to 0.4-1Pa; Open hydrogen or argon gas that gas meter charges into 200-600Pa then; Start the voltage of 500-700V, utilize high-voltage to be heated to 500-650 ℃, ion bombardment steel surface decomposition compound layer with ionization of gas and with sample; Insulation 4-12h; In 3-5 minute, gas flow is reduced to zero then, remove voltage, steel sample naturally cools to room temperature;
The steel sample that (3) will pass through ion bombardment in the making Nano surface trier of packing into, carries out Surface Nanocrystalline to steel surface after ultrasonic cleaning; With diameter is the bottom that the Cr15 steel ball of 3-8mm is placed on the sample chamber; Steel ball is 28-40mm apart from the steel sample surface, and the ultrasonic vibration frequency that the head that shakes is set is 20KHz, drives steel ball through ultrasonic vibration the steel sample surface is clashed into; Treatment time is 2-4h; Obtaining the top layer on the steel sample surface at last is the pure diffusion layer tissue of nano-scale, its hardness >=1240HV, and nitriding fragility is 1 grade.
2. the surface treatment method of a kind of ferrous materials nitrided case according to claim 1 is characterized in that described nitriding steel comprises 20CrMo steel and 38CrMoAl steel.
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| WO2014190908A1 (en) * | 2013-05-30 | 2014-12-04 | 先健科技(深圳)有限公司 | Manufacturing method of iron-based alloy medical apparatus |
| CN106521123A (en) * | 2016-12-09 | 2017-03-22 | 四川大学 | Material surface modification device and method |
| CN106947937A (en) * | 2017-03-13 | 2017-07-14 | 辽宁石油化工大学 | A kind of preparation method for the steel stirring friction welding agitator head that ionic nitriding surface is modified |
| CN109183020A (en) * | 2018-08-27 | 2019-01-11 | 合肥工业大学 | A kind of preparation method of aluminum alloy surface complex gradient modified layer |
| CN114574800A (en) * | 2022-02-17 | 2022-06-03 | 合肥力和机械有限公司 | Micro steel ball and surface carburizing and hardening coordination treatment process |
| CN115609241A (en) * | 2022-11-01 | 2023-01-17 | 安徽省含山县威建铸造厂(普通合伙) | Processing method for improving unstable fatigue life of spring |
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| CN104207866A (en) * | 2013-05-30 | 2014-12-17 | 先健科技(深圳)有限公司 | Manufacturing method for medical apparatus capable of being absorbed by organism or for absorbable part of medical apparatus |
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| CN106521123A (en) * | 2016-12-09 | 2017-03-22 | 四川大学 | Material surface modification device and method |
| CN106947937A (en) * | 2017-03-13 | 2017-07-14 | 辽宁石油化工大学 | A kind of preparation method for the steel stirring friction welding agitator head that ionic nitriding surface is modified |
| CN109183020A (en) * | 2018-08-27 | 2019-01-11 | 合肥工业大学 | A kind of preparation method of aluminum alloy surface complex gradient modified layer |
| CN114574800A (en) * | 2022-02-17 | 2022-06-03 | 合肥力和机械有限公司 | Micro steel ball and surface carburizing and hardening coordination treatment process |
| CN114574800B (en) * | 2022-02-17 | 2023-12-01 | 合肥力和机械有限公司 | Miniature steel ball and surface carburization and hardening coordination treatment process |
| CN115609241A (en) * | 2022-11-01 | 2023-01-17 | 安徽省含山县威建铸造厂(普通合伙) | Processing method for improving unstable fatigue life of spring |
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Application publication date: 20120711 |