CN104988288A - No-hydrogen atmosphere protection heat treatment process completely without decarburization for steel - Google Patents
No-hydrogen atmosphere protection heat treatment process completely without decarburization for steel Download PDFInfo
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- CN104988288A CN104988288A CN201510451323.7A CN201510451323A CN104988288A CN 104988288 A CN104988288 A CN 104988288A CN 201510451323 A CN201510451323 A CN 201510451323A CN 104988288 A CN104988288 A CN 104988288A
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Abstract
The invention discloses a no-hydrogen atmosphere protection heat treatment process completely without decarburization for steel. CO2 is fed in a gas generation furnace with activated carbons, and is chemically reacted with the activated carbons; a reaction product a is fed in a sealing atmosphere furnace with workpieces to be thermally treated; then, N2 is fed in the sealing atmosphere furnace to dilute the reaction product a; the contents of the reaction product a and N2 in the sealing atmosphere furnace are adjusted through comparing a set value of a carbon controller with a carbon potential measurement value in the atmosphere in the sealing atmosphere furnace to form a no-hydrogen protection atmosphere; the workpieces can be located in the no-hydrogen environment in the heating and insulation process of the heat treatment; the carbon potential in the atmosphere is always kept the same with the carbon content of the workpieces in the furnace; the workpieces generate no decarburization or recarburization through long-time stop under high temperature; the complete protection of the steel in the no-hydrogen environment is realized; and the decarburization problem of large and ultralarge workpieces manufactured by high-strength steel and ultrahigh-strength steel in the heat treatment in the field of aerospace is solved.
Description
Technical field
The present invention relates to the atmosphere protection of metallic substance heat-treated steel, be specifically related to one and steel part can be made to be in without hydrogen environment in heat treated heating and insulating process, and without the heat-treatment technology method of decarburization phenomenon.
Background technology
To in steel components heat treatment process, in order to prevent workpiece at high temperature decarburization and oxidation, generally all adopting vacuum heat treatment or using protective atmosphere to process in the atmosphere furnace of sealing.Conventional protective atmosphere has inert atmosphere (as nitrogen, argon gas etc.), nitrogen and Carbinol atmosphere, dissociated methanol gas, RX gas, nitrogen-based atmosphere etc.
At high temperature can not there is chemical reaction with workpiece material in rare gas element, but unavoidable containing other foreign gases in usual rare gas element, as O
2, CO
2, H
2o etc.In practice, even if rare gas element reaches very high purity (foreign gas is at below 5ppm), applying such rare gas element, is also at high temperature very limited to the protection of steel workpiece.The workpiece of such as 30CrMnSi material was 900 DEG C of insulations 1 hour, and the high pure nitrogen with 99.9997% is as protection gas, and the zone of oxidation of workpiece surface is greater than 0.1mm, and Decarburized layer is more above 0.5mm.Therefore under high temperature, the protected effect of rare gas element is not good.
Nitrogen and Carbinol atmosphere and RX gas are normally as the basic atmosphere of carburizing atmosphere, and its component is probably CO:20-25%; H
2: 35-45%, a small amount of H
2o and CO
2(less than 2%), all the other are N
2.This protective atmosphere also adds acetone, propane, methane etc. as enriched gas usually to improve carbon potential, also adds air if desired to reduce carbon potential, thus realizes the carbon potential required for technique.These two kinds of protective atmospheres can as excellent carburizing atmosphere, can certainly as the protective atmosphere of steel.Because this carbon-potential control technology is very ripe and reliable, so workpiece can realize the protection completely without decarburization and oxidation under this protective atmosphere, namely protect completely.Other carburizing atmosphere also all possesses same character.But because the equipment cost of carburizing atmosphere and running cost slightly high, be all for carburization process usually, be applied in the few of protective atmosphere technique.
Nitrogen-based atmosphere is with high-purity N
2based on a kind of protective atmosphere.In order to improve N
2protective capability, at N
2in add a small amount of reducing gas, as propane, methane, CO etc.Propane, methane enter in stove and at high temperature decompose, and produce strong reducing property gas H
2and CO.In nitrogen-based atmosphere, the volume ratio of reducing gas is generally below 5%, maximum also can not more than 8%.At high temperature workpiece can anti-oxidation in this this atmosphere, but has decarburization to a certain degree.The workpiece of 30CrMnSi material 900 DEG C of insulations 1 hour, the high pure nitrogen with 99.9997% and 5% CO gas mixture as protecting gas, the basic non-oxidation of workpiece surface, but have 0.2 ~ 0.3mm Decarburized layer.If less demanding to the Decarburized layer of workpiece surface, the protective atmosphere very desirable really of nitrogen-based atmosphere.Nitrogen-based atmosphere compares the equipment cost of carburizing atmosphere in addition and running cost is all lower, and also less, security is higher for the reducing gas contained in atmosphere, and control climate is simple, so in the atmosphere protection technique of steel workpiece, nitrogen-based atmosphere application is more extensive.
The high-strength steel that aerospace field is conventional and ultrahigh-strength steel, as 30CrMnSiA, 40CrNiMo, 30CrMnSiNi2A etc., due to responsive to hydrogen embrittlement, so can not contain hydrogen in claimed atmosphere.Like this, nitrogen and Carbinol atmosphere, RX gas and other carburizing atmosphere, all because wherein can not use containing a large amount of hydrogen.In order to avoid hydrogen embrittlement and decarburization, at present, the part that the high-strength steel not too large for size or ultrahigh-strength steel are made, generally all adopts vacuum heat treatment, requires that Decarburized layer is not more than 0.075mm.Certain Decarburized layer is the smaller the better.But at aerospace field, some workpiece sizes are beyond the use range of conventional vacuum oven.And vacuum oven is along with the increase of size, the total pressure of not only bearing because of the increase of volume is increasing, require thicker stronger furnace wall, and obtain needed for vacuum tightness more next difficult, so vacuum oven is along with the increase of size, not only equipment cost is more and more higher, exponentially increase, be also difficult to reach required vacuum tightness.So the super spare parts (as rocket body) of space industry, does not generally have sfgd., namely can only thermal treatment in air furnace, let alone decarburization.After heat treatment, blast is adopted to remove oxidation and decarbonization layer.For the aerospace parts of oversize, it is not only very difficult that blast removes Decarburized layer, and the depth removing Decarburized layer is restive.Decarburized layer may cause workpiece surface tensile stress, and Decarburized layer hardness is low, and the strength of materials significantly declines, and the intensity of part and dimensional precision all can be subject to obvious impact, and the quality risk of part is increased.
In recent years, there is producer to attempt using the nitrogen-based atmosphere of the CO containing 5% as protective atmosphere, process the large-scale part in aerospace field.This atmosphere is based on high-purity rare gas element; add the CO of a small amount of constant; not hydrogen in atmosphere, it also has certain effect to the protection of this type of part, but; it to the protected effect of workpiece as mentioned above; it is not bad to the protection of oxidation, but the protection of decarburization is not very desirable, and general decarburized layer deepness is all at 0.2 ~ 0.3mm; and carbon loss in Decarburized layer is serious, hardness and strength degradation remarkable.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of this invention is to provide a kind of heat-treatment technology method, in the atmosphere furnace of sealing, setting up no hydrogen atmosphere, by regulating the N passed in stove
2with CO and CO
2the flow of gas mixture and ratio; the carbon potential of atmosphere is made to remain equal with the carbon content of workpiece in stove; thus realize workpiece and at high temperature to stop for a long time and can not decarburization or carburetting; solve the decarburization problem during thermal treatment of the large-scale and ultra-large workpiece that aerospace field is made up of high-strength steel and ultrahigh-strength steel, realize the protection completely without the steel of hydrogen environment.
To achieve these goals, the technical solution used in the present invention is:
The complete protection of the no hydrogen atmosphere without a decarburization thermal treatment process for steel, by CO
2pass into gac is housed carbide feed generator in and with gac generation chemical reaction, reaction product a is passed into and is placed with in the sealing atmosphere furnace of workpiece to be heated, then to sealing atmosphere furnace in pass into N
2diluting reaction product a, by the set(ting)value of carbon control instrument and the contrast of the carbon potential measurement value of sealing atmosphere furnace atmosphere, regulates sealing atmosphere reaction in furnace product a and N
2content, makes the carbon potential of the atmosphere in sealing atmosphere furnace equal with the carbon potential of steel part to be heated.
Described CO
2the temperature that chemical reaction occurs in carbide feed generator with gac is 800 ~ 1000 DEG C, and preferable temperature is higher than sealing atmosphere furnace temperature 30 DEG C.Such as the workpiece of 30CrNnSi material, its sealing atmosphere furnace in technological temperature be generally 900 DEG C, then the preferable temperature of carbide feed generator is 930 DEG C.
Described CO
2be CO and CO with gac reaction product a
2mixed gas, wherein CO
2content is 1% ~ 6%, and all the other are CO.
The described N passed in sealing atmosphere furnace
2purity be not less than 99.95%.
Described sealing atmosphere furnace is provided with thermopair, gas analyzer and oxygen probe or Lang Muda probe, measures the temperature of sealing atmosphere furnace, CO content and CO respectively
2content and oxygen gesture, measure parameter, and just can be calculated the observed value of atmosphere carbon potential by the carbon potential software for calculation of carbon control instrument or specialty, described carbon control instrument can select Continental Europe 2604 or 2704 controller.
The set(ting)value of described carbon control instrument chooses the nominal carbon content of steel part to be heated in sealing atmosphere furnace.
The observed value of the atmosphere carbon potential that described carbon control instrument shows can adopt the carbon potential calibration steps in carburization process to calibrate, and described carbon potential calibration steps can adopt pool sheet weighting method or peeling method.
The set(ting)value of described carbon control instrument can do corresponding fine setting according to the measuring result of the real test of technique, and surface of test piece carburetting, setting point is to low-key, and surface of test piece decarburization, setting point is to rise, and described amount trimmed is not more than 20%.
Atmosphere ratio in described sealing atmosphere furnace by mole mass ratio is: CO:20 ~ 90%, CO
2: 0 ~ 8%, all the other are N
2.
The invention has the beneficial effects as follows:
1) CO is adopted
2with the chemical reaction product of gac as the main ingredient of protective atmosphere, obtain the high carbon potential atmosphere of not hydrogen easily, and then give in atmosphere and pass into N2 to dilute atmosphere, for the control of the carbon potential carrying out no hydrogen atmosphere creates condition.
2) adopt the mode of carbon-potential control to regulate atmosphere without hydrogen protective atmosphere, make the anti-decarburization protection of workpiece in no hydrogen atmosphere reach unprecedented level.
3) set(ting)value of atmosphere carbon-potential control is the nominal carbon content of the material of workpiece.Adopt the workpiece of this rule process, its surface carbon content can be close to atmosphere carbon potential gradually, that is no matter the actual carbon content of workpiece material is how many, and after this technological process, the carbon content of workpiece surface can the nominal carbon content of convergence and this material national regulations.Such as workpiece material is 30CrMnSiA, and the setting point of atmosphere carbon potential is 0.30%, and the surface carbon content of the workpiece of process also will be 0.30%;
4) not hydrogen in the protective atmosphere component of this programme, avoids the generation of hydrogen embrittlement, is applicable to the most basic demand of the heat-treating atmosphere protection of high-strength steel and ultrahigh-strength steel.
5) protective atmosphere of this programme is suitable for high-strength steel and the anti-decarburization of superstrength Heat Treatment Of Steel and oxidizing process very much, can certainly be used for the thermal treatment anti-oxidation decarburizing protection of other steel components, for Heat Treatment Of Steel protection provides a kind of novel method.
6) atmosphere furnace that have employed sealing of this programme is as the equipment processing workpiece, atmosphere furnace is not substantially by limitation of size, can have made to order according to the size of workpiece, so all can process large-scale and superhuge aerospace parts, thoroughly solve current this kind of part and cannot protect the present situation letting alone decarburization oxidation, all will produce great effect for the loss of weight of aerospacecraft and safety coefficient.
7) the equipment cost investment of the use of this programme is low, economic benefits, and the several times of the atmosphere furnace that the price due to isometric vacuum oven seals often, so adopt the present invention, equipment investment cost significantly declines.
8) this programme is better than vacuum oven to the protection effect of decarburization.The protection effect of vacuum oven is relevant with vacuum tightness.The vacuum tightness obtained under current technical qualification, its protection effect can make the Decarburized layer of steel be not more than 0.075mm.And the principle of the carbon potentials such as employing of the present invention, can accomplish completely without decarburization.
9) protective atmosphere of this programme, it is much better than nitrogen-based atmosphere (from the test result contrast of Fig. 5 and Fig. 6 clearly) to the protection effect of steel when thermal treatment.
10) this processing method is domestic initiation, occupies advanced international standard.
Accompanying drawing explanation
Fig. 1 is implementing process schematic flow sheet of the present invention.
Fig. 2 is that gas mixture of the present invention passes in the atmosphere furnace of sealing, CO
2in 2%, 4% and 6% situation, the graph of a relation of CO content and carbon potential.
Fig. 3 is CO:CO of the present invention
2under=35:1 condition, carbon potential when 900 DEG C and the relation between gas mixture accounting.
Fig. 4 is the conditional curve of heat treatment process test of the present invention, and wherein red line is temperature curve, blue line is CO content, green line is carbon potential in stove.
Fig. 5 is the hardness gradient curve of the 30CrMnSi specimen surface of protective atmosphere process of the present invention.
Fig. 6 is that the present invention adopts nitrogen-based atmosphere containing 5%CO as the surface hardness gradient curve of the 30CrMnSi sample of protective atmosphere process.
Wherein, 1, nitrogen storing apparatus, 2, CO2 storing apparatus, 3, gas analyzer, 4, furnace gas air delivering pipeline, 5, furnace atmosphere, 6, workpiece in stove, 7, thermopair, 8, oxygen probe, 9, the atmosphere furnace of sealing, 10, nitrogen magnetic valve, 11, CO magnetic valve, 12, CO pressure converter, 13, thermopair, 14, gac, 15, carbide feed generator, 16, CO2 pressure converter, 17, nitrogen pressure umformer.
Embodiment
Below in conjunction with concrete enforcement, the present invention is described further.The present invention's test first on the large-scale associating electric furnace of Xi'an Aircraft Manufacturing Corporation succeeds.Furnace volume is about 35M
3, main process material is 30CrMnSiA, 30CrMnSiNi2,40CrNiMo, the large aerospace parts such as 4140.Sample is diameter phi 12, and length is the cylinder of 10mm, tests and all tests above-mentioned 4 kinds of materials.
As shown in Figure 1, a kind of complete protection of the no hydrogen atmosphere without decarburization thermal treatment process of steel, implemented by following steps:
1) raw material is solid activated carbon (particulate state), CO
2gas and N
2, by CO
2and N
2be stored in CO respectively
2in storing apparatus 2 and nitrogen storing apparatus 1, gac is contained in carbide feed generator 15;
2) unstripped gas CO
2from CO
2storing apparatus 2 flows out, be decompressed to through pressure converter 16 and send into carbide feed generator 15 after 0.01 ~ 0.2MPa and react with gac 14, after the temperature of gac 14 is detected by thermopair 13, the temperature of gac 14 controls at 930 DEG C by Controlling System, is resultant CO and a small amount of unreacted CO from carbide feed generator 15 gas out
2mixed gas;
3) mixed gas of step 2 enters the atmosphere furnace 9 of sealing, and controls its uninterrupted or break-make through CO magnetic valve 11 after being decreased to 5KPa by CO pressure converter 12 pressure;
4) atmosphere data collection, is obtained temperature (DEG C), oxygen gesture (mV), CO and CO of current ambiance respectively by thermopair 7 oxygen probe 8 in the atmosphere furnace 9 sealed and gas analyzer 3
2content (%);
5) according to the temperature (DEG C) in stove, oxygen gesture (mV), CO and CO
2content (%), by the carbon control module of carbon control instrument, or by computer, special carbon potential software for calculation is installed, just can obtains the theoretical carbon potential of atmosphere;
6) according to the carbon determination method generally adopted during carbon potential calibration in carburization process, the carbon potential that theory obtains is calibrated, obtain the observed value of the carbon potential of protective atmosphere; Carbon content according to workpiece chooses the set(ting)value of the carbon potential of protective atmosphere, and carbon potential set(ting)value selects the nominal carbon content of workpiece material, and carbon amounts can do corresponding fine setting; Such as 30CrMnSi, name carbon content is 0.3%, carbon potential setting point just selects 0.3%c, usually adopt and just can meet the demands in this way, if can not meet the demands, then need slightly to adjust setting point, if such as 40CrNiMo selects 0.4%c as the setting point of atmosphere carbon potential, workpiece surface can slight carburetting, and after being adjusted to 0.36%c, workpiece surface is without carburetting and decarburization phenomenon.
7) by comparing set(ting)value and the actual value of atmosphere carbon potential, by unstripped gas N
2flowed out by nitrogen storing apparatus 1, pass into interior dilution CO and the CO of atmosphere furnace 9 of sealing
2gas mixture; its uninterrupted or break-make is controlled by nitrogen magnetic valve 10 after nitrogen pressure umformer 17 pressure alteration; control nitrogen magnetic valve 10 and CO magnetic valve 11 carry out the content of CO in adjustments of gas producer 15; when carbon potential actual value is higher than set(ting)value; open or increase nitrogen magnetic valve 10; reduce or close CO magnetic valve 11; when actual carbon potential value is lower than set(ting)value; reduce or close nitrogen magnetic valve 10; open or increase CO magnetic valve 11, making the actual value of the carbon potential of protective atmosphere remain consistent with the set(ting)value of carbon potential.
The parameter of technological test is as table 1.
Checked in Xi'an Aircraft Manufacturing Corporation by the sample of above process parameter test, all sample Decarburized layers meet the requirement being not more than 0.075mm.
As shown in Figure 4, the conditional curve of heat treatment process test, wherein red line is temperature curve, blue line is CO content, green line is carbon potential in stove.
As shown in Figure 5, the hardness gradient curve of protective atmosphere process 30CrMnSi specimen surface.
As shown in Figure 6, adopt the nitrogen-based atmosphere containing 5%CO as the surface hardness gradient curve of the 30CrMnSi sample of protective atmosphere process.
The scope that protective atmosphere of the present invention is suitable for is not limited to these the 4 kinds of materials disclosed in test; also high-strength steel and superstrength steel is not limited to; although original intention of the present invention is the decarburization problem solving this kind of material; if the metal of other any carbon containings has decarburization phenomenon when thermal treatment, this protective atmosphere all can be adopted to protect.
Claims (9)
1. the complete protection of the no hydrogen atmosphere without a decarburization thermal treatment process for steel, is characterized in that, by CO
2pass into gac is housed carbide feed generator in and with gac generation chemical reaction, reaction product a is passed into and is placed with in the sealing atmosphere furnace of workpiece to be heated, then to sealing atmosphere furnace in pass into N
2diluting reaction product a, by the set(ting)value of carbon control instrument and the contrast of the carbon potential measurement value of sealing atmosphere furnace atmosphere, regulates sealing atmosphere reaction in furnace product a and N
2content, makes the carbon potential of the atmosphere in sealing atmosphere furnace equal with the carbon potential of steel part to be heated.
2. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1, is characterized in that, described CO
2the temperature that chemical reaction occurs in carbide feed generator with gac is 800 ~ 1000 DEG C, and preferable temperature is higher than sealing atmosphere furnace temperature 30 DEG C.
3. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1, is characterized in that, described CO
2be CO and CO with gac reaction product a
2mixed gas, wherein CO
2content is 1% ~ 6%, and all the other are CO.
4. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1, is characterized in that, the described N passed in sealing atmosphere furnace
2purity be not less than 99.95%.
5. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1; it is characterized in that; described sealing atmosphere furnace is provided with thermopair, gas analyzer and oxygen probe or Lang Muda probe, measures the temperature of sealing atmosphere furnace, CO content and CO respectively
2content and oxygen gesture, measure parameter, and just can be calculated the observed value of atmosphere carbon potential by the carbon potential software for calculation of carbon control instrument or specialty, described carbon control instrument can select Continental Europe 2604 or 2704 controller.
6. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1, it is characterized in that, the set(ting)value of described carbon control instrument chooses the nominal carbon content of workpiece to be heated in sealing atmosphere furnace.
7. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1; it is characterized in that; the observed value of the atmosphere carbon potential that described carbon control instrument shows can adopt the carbon potential calibration steps in carburization process to calibrate, and described carbon potential calibration steps can adopt pool sheet weighting method or peeling method.
8. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1; it is characterized in that; the set(ting)value of described carbon control instrument can do corresponding fine setting according to the test result of technological test; surface of test piece carburetting; setting point is to low-key; surface of test piece decarburization, setting point is to rise, and described amount trimmed is not more than 20%.
9. the complete protection of the no hydrogen atmosphere without the decarburization thermal treatment process of a kind of steel according to claim 1, it is characterized in that, the atmosphere ratio in the atmosphere furnace of described sealing is in molar ratio: CO:20 ~ 90%, CO
2: 0 ~ 8%, all the other are N
2.
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Cited By (6)
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| CN111020141A (en) * | 2019-12-03 | 2020-04-17 | 上海丰东热处理工程有限公司 | Atmosphere-controllable heat treatment processing technology |
| CN111644130A (en) * | 2020-06-28 | 2020-09-11 | 朗瑞(泰州)金属工具有限公司 | Method for manufacturing pipe orifice for glass lining equipment |
| CN112609056A (en) * | 2021-01-07 | 2021-04-06 | 湖北中冶窑炉有限公司 | Decarburization-preventing steel through type heat treatment system and heat treatment method |
| CN112921160A (en) * | 2021-01-14 | 2021-06-08 | 广东世创金属科技股份有限公司 | Low-hydrogen or hydrogen-free controllable atmosphere for metal heat treatment and preparation method and application thereof |
| CN113981186A (en) * | 2021-09-23 | 2022-01-28 | 浙商中拓集团(浙江)新材料科技有限公司 | Atmosphere protection heat treatment process for preventing decarbonization and recarburization |
| WO2024021560A1 (en) * | 2022-07-28 | 2024-02-01 | 苏州普热斯勒先进成型技术有限公司 | Device and method for manufacturing hot-stamped part |
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| WO2024021560A1 (en) * | 2022-07-28 | 2024-02-01 | 苏州普热斯勒先进成型技术有限公司 | Device and method for manufacturing hot-stamped part |
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