Research progress on austenite grain growth and second-phase particle control technology in automotive gear steel
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摘要: 伴隨著全球雙碳政策的實施，節能減排成為汽車制造業發展的首要目標之一. 汽車用齒輪鋼采用的更高溫度結合更短時間的滲碳工藝是目前各齒輪生產企業最為直接的降碳措施，但齒輪鋼在高溫滲碳生產過程中卻時常發生奧氏體晶粒異常粗大的問題，且滲碳溫度越高混晶現象越嚴重. 因此，各企業對齒輪鋼進行微合金化，通過添加微合金元素在加熱過程中析出第二相粒子產生釘扎作用來阻礙奧氏體晶粒異常長大，從而需要對復雜的齒輪鋼奧氏體晶粒長大與第二相粒子析出機制進行研究. 通過對奧氏體晶粒度、奧氏體晶粒長大機制及模型、第二相粒子(Nb(C,N)/AlN)對奧氏體晶界移動的釘扎作用及模型、以及加熱溫度與保溫時間對奧氏體晶粒長大和第二相粒子釘扎作用的影響等進行了文獻綜述，闡明了奧氏體晶粒長大規律、第二相粒子的控制方法與抑制奧氏體晶粒長大的釘扎機制，為高質量齒輪鋼的生產提供參考.Abstract: With the implementation of the global two-carbon policy, energy saving and CO2 emission reduction have become important developmental goals of the automobile manufacturing industry. At present, the combination of high temperature for the automobile gear steel and short carburizing time is the most direct carbon reduction countermeasure for gear production enterprises. However, the problem of abnormally coarsened austenite grains often occurs in the high-temperature carburization of gear steel. With the increase in carburizing temperature, the degree of mixing crystals becomes serious. As a requirement of gear manufacturing enterprises, microalloying is carried out on the carburized gear steel. Upon the addition of microalloying elements, the second-phase particles are precipitated during heating, and the pinning effect is generated to prevent the movement of austenite grain boundaries, thus preventing the abnormal growth of austenite grains. Although the second-phase particles precipitate at the usual carburizing temperature, the partial solid solution of particles appears. In this work, the effects of the heating temperature and holding time on the austenite grain size of gear steel are studied to clarify the mechanisms of complex austenite grain growth and second-phase particle precipitation for the realization of fine austenite grain size after high-temperature carburization. The influence of the contents of microalloying elements (Nb, Al) on the pinning effect, precipitation position, and solution temperature of the second-phase particles (Nb (C, N)/AlN) are also discussed. Austenite grain growth models, critical sizes of austenite grain abnormal growth, and pinning force models of second-phase particles are summarized. The austenite grain growth model is based on the Beck equation, and the most common models are the modified Sellars and Arrhenius models. For the study of the inhibition effect on austenite grains, the pinning force model is used to study the critical size of austenite by modifying the dimensionless constant (A) of the Zener equation mainly through the pinning effect (Pz) produced by all particles on the grain boundary. After the experimental data are obtained, the trend of austenite growth can be predicted accurately by fitting the curve using the mathematical method. The precipitated second-phase particles are generally distributed along the grain boundary. Nb (C, N) particles have a higher solution temperature than AlN particles, so they are more stable at high temperatures. When the temperature exceeds the grain coarsening temperature, the precipitated particles become dissolved or coarsened. The mixed crystal structure generally starts to appear at about 1000 ℃, and adding the appropriate amount of microalloying elements can increase the coarsening temperature.
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Key words:
- gear steel /
- austenite grain size /
- abnormal growth /
- second-phase particle /
- mixed crystal /
- pining force
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圖 5 在1000 °C加熱1 h后的奧氏體晶粒形貌. (a) 無Nb鋼; (b) Nb微合金鋼
Figure 5. Austenite grain morphology after heating at 1000 ℃ for 1 h: (a) Nb-free steel; (b) Nb-microalloyed steel
圖 6 850 ℃和950 ℃下試驗鋼中析出相的EPMA圖譜結果
Figure 6. EPMA mapping results of phases precipitated in test steel at 850 and 950 ℃
圖 10 1250 ℃時，未溶解碳氮化物粒子的透射電鏡觀察圖
Figure 10. TEM diagram of undissolved carbonitride particles at 1250 ℃
圖 13 含Nb的第二相粒子在晶界的分布
Figure 13. Distribution of Nb containing second phase particles along grain boundaries
圖 15 NbC和AlN質量分數隨奧氏體化溫度(tγ)的變化
Figure 15. Variation of NbC and AlN mass fraction withaustenitizing temperature
圖 17 晶界和球形粒子之間相互作用的示意圖. (a)未接觸；(b)接觸
Figure 17. Schematic of the interaction between grain boundaries and spherical particles: (a) no contact；(b) with contact
圖 19 偽滲碳后奧氏體晶粒粗化情況與鋼中析出粒子釘扎強度間的關系[48]
Figure 19. Relationship between average austenite grain size and pinning strength after pseudocarburization
圖 20 初始晶粒尺寸及釘扎力與晶粒長大模式間的關系[48]
Figure 20. Grain growth regimes as functions of prior grain size and pinning force
圖 21 溫度對奧氏體晶粒與析出相的影響[81]. (a) 奧氏體晶粒尺寸隨加熱溫度的變化; (b) 850 ℃溫度下析出相; (c) 1150 ℃溫度下析出相; (d) 1250 ℃溫度下析出相
Figure 21. The effect of temperature on austenite grain and precipitated phase[81]: (a) change of austenite grain size with heating temperature; (b) precipitated phase at 850 ℃; (c) precipitated phase at 1150 ℃; (d) precipitated phase at 1250 ℃
圖 23 無Nb，質量分數為0.021%的Nb微合金20MnCr5鋼在800～1250 ℃加熱1 h后的奧氏體晶粒形貌
Figure 23. Austenite grain morphology of Nb-free and mass fraction of 0.021% Nb-microalloyed 20MnCr5 samples heated at 800–1250 ℃ for 1 h
圖 24 奧氏體長大和混晶組織的演變過程
Figure 24. Evolution of austenite growth and mixed grain structure
表 1 20MnCr5鋼的化學成分標準(質量分數)
Table 1. Standard chemical composition of 20MnCr5 steel (mass fraction)
% C Mn Cr Ni Mo Nb Si Al 0.17–0.22 1.10–1.40 1.00–1.30 ≤0.25 ≤0.03 trace ≤0.18 0.02–0.05 
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表 2 奧氏體晶粒長大模型
Table 2. Austenite grain growth models
Author and publication Unit Material Equation Brief description Beck et al.[12] Notre Dame University High purity aluminum $ D = {D_{\text{0}}} \cdot {t^n} $ Relationship between austenite grain size and holding time at a certain heating temperature. Hillert[13] Royal Polytechnic $ {D^2} = D_0^2 + C \cdot t $ Relationship among austenite grain growth and temperature and time Hu and Rath[16] American Steel Company $ {D^{\left(1/n\right)}} = D_0^{\left(1/n\right)} + K \cdot t $ Isothermal grain growth kinetics, n and K, are the growth index and rate constant, respectively. Sellars and Whiteman[14] Sheffield University Low-carbon manganese steel $ {D^n} = D_0^n + {K_0} \cdot \exp \left( - \dfrac{Q}{{RT}}\right) \cdot t $ Most existing empirical models for austenite grain growth are based on this study. Nishizawa[17] Tohoku University, Japan High purity iron $ {D^2} = D_0^2 + C \cdot t $ $ C = \dfrac{{\sigma V{D_{{\text{gb}}}}}}{{\lambda RT}} $ Jiao et al.[18] Ghent University Si?Mn steel $ {D^n} = D_0^n + {K_1} \cdot \exp \left(\dfrac{{{K_2}}}{T}\right) \cdot t $ K1, K2, and n are related to temperature. Moon et al.[19] POSCO C?Mn steel $ \dfrac{{{\text{d}}D}}{{{\text{d}}t}} = n \cdot K \cdot {\left(\dfrac{1}{D}\right)^{\left(\frac{1}{n}\right)}}^{ - 1} $ According to Hu’s model[16], the equation of grain growth rate is obtained by the differential method. Yue et al.[20] Northeast Special Steel GCr15 $ {D^n} = D_0^n + {K_0} \cdot \exp \left( - \dfrac{Q}{{RT}}\right) \cdot t $ Coefficients K0 and n and activation energy Q in the model have different values for various steel grades and transformation stages. Lee and Lee[15] Yonsei University Cr?Mo steel $ D = K \cdot {t^n} $ K is expressed by Arrhenius equation:
$ K = {K_0} \cdot \exp \left( - \dfrac{Q}{{RT}}\right) $.Zhu et al.[21] Beijing University of Science and Technology Carburized bearing steel SAE8620H $ {D^n} = {K_0} \cdot \exp \left( - \dfrac{Q}{{RT}}\right) \cdot t $ When D0 is ignored, the simplified Sellars model is the most accurate, and the correlation between the predicted value and the experimental value is the highest. Yang et al.[22] Angang Steel Group Limited 18CrNiMo7-6 $ D = {K_0} \cdot \exp \left( - \dfrac{Q}{{RT}}\right) \cdot {t^n} $ When D>3D0, D0 can be ignored. Yang et al.[23] Central Iron & Steel Research Institute 20CrMnTiNb $ {D^2} = D_0^2 + C \cdot \exp \left( - \dfrac{Q}{{RT}}\right) \cdot t $ Comparison of grain growth between Nb-containing and Nb-free 20CrMnTi steel samples by Hillert model Bao et al.[24] Wuhan University of Science and Technology Medium manganese martensitic wear-resistant steel NM500 $ D = {K_0} \cdot \exp \left( - \dfrac{Q}{{RT}}\right) \cdot {t^n} $ When the temperature is less than 950 ℃, n is relatively small, and the experimental data are close to the predicted value. He et al.[25] Xining Special Steel Plant 20MnCr5 $ {D^2} = D_0^2 + C \cdot \exp \left( - \dfrac{Q}{{RT}}\right) \cdot t $ This model is applicable to normal grain growth.
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表 3 奧氏體晶粒臨界尺寸的研究
Table 3. Studies on the critical grain size of austenite
Author and publication Unit Material Equation (R0) Brief description Smith[27] University of Chicago High purity aluminum $ A \cdot \dfrac{r}{f} $ $ A = \dfrac{4}{3} $, general form: $ A \cdot \dfrac{r}{{{f^m}}} $. Hillert[13] Royal Polytechnic $ \dfrac{{4r}}{{9f}}\left(\min \right)/\dfrac{{2r}}{{3f}}\left(\max \right) $ When R reaches the lower limit, the grains will stop growing normally and begin to grow abnormally until the upper limit value is reached. Gladman[26] United Steel $ \left[\pi \cdot \left(\dfrac{1}{4} - \dfrac{1}{{3Z}}\right)\right] \cdot \dfrac{r}{f} $ Z is the nonuniformity factor representing the particle size distribution. When Z ≤ 4/3, grain growth is inhibited. Haroun and Budworth[28]
Sheffield University $ 1.03 \cdot \dfrac{r}{{{f^{0.5}}}} $ Modified Zener equation under the condition that at least one particle exists at each grain boundary. Nes et al.[29] Norwegian Institute of Technology $ 1.54 \cdot \dfrac{r}{{{f^{0.92}}}} $ Considering the influence of particle shape and distribution. Elst et al.[30] Philips Copper alloy $ \dfrac{{2\beta }}{3} \cdot \left(\dfrac{3}{2} - \dfrac{2}{Z}\right) \cdot \dfrac{r}{f} $ The bimodal grains and the particles precipitated at the grain boundary are calculated; β is a function of R0/r. Rios[31] Volta Redonda Steel $ 0.33 \cdot \dfrac{r}{f} $ Derived based on three different methods. Kad and Hazzledine[32] University of California $ 1.41 \cdot \dfrac{r}{{{f^{0.5}}}} $ Simulation results of square and hexagonal lattices reveal the diffusion of particles with special shapes \left(sphere, needle, and plate\right). Moon et al.[33] Hanyang University TiN Steel $ 1.5 \cdot \dfrac{r}{f} $ The Zener coefficient of TiN particles is 1.5. Zhou et al.[34] Wuhan University of Science and Technology 38CrMoAl $ A \cdot \dfrac{r}{f} $ A is about 0.17 when the grains grow normally. Moon and Lee[35] Korea Institute of Materials TiN Steel $ 1.33 \cdot \dfrac{r}{f} $ The second-phase particles must be fine and have a high volume fraction to effectively pin the grains. Xu et al.[9] Daye Special Steel SAE4320 $ A \cdot \dfrac{r}{f} $ When the temperature is kept below Ac3 temperature, the precipitated second-phase particles will not dissolve, and Ostwald will ripen. As a result, grain growth is inhibited. Ma et al.[36] Beijing University of Science and Technology 20CrMnTi $ 0.1694 \cdot \dfrac{r}{f} $ The grain radius is controlled to be less than the critical radius, and the grain grows normally. Qi and Li[37] Hebei Iron and Steel 20MnCr5 $ A \cdot \dfrac{r}{f} $ With the increase in temperature and holding time, the number of second-phase particles decreases, and the pinning effect on the grain boundary gradually weakens. Guo et al.[38] Zhengzhou University X80M Steel $ \pi \cdot \left(\dfrac{1}{4} - \dfrac{1}{{3Z}}\right) \cdot \dfrac{r}{f} $ The normal Z value of general metal materials is about 1.7.
Li et al.[39] Beijing University of Science and Technology 20CrMnTi $ \dfrac{{\pi r}}{{6f}} \cdot \left(\dfrac{3}{2} - \dfrac{2}{Z}\right) $ The grain boundary is pinned by the precipitated second-phase nanoparticles.
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表 4 元素對奧氏體晶粒長大的作用
Table 4. Effect of various elements on austenite grain growth
Element Effect C, Mn and P Promote growth Si, N and Cu Weak inhibition Mo, Cr and W Moderate inhibition Nb, V, Ti, Al, Zr, N and O Strong inhibition
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表 5 Al含量對奧氏體晶粒尺寸的影響
Table 5. Effect of Al content on austenite grain size
Author and publication Unit Steel Brief description Dong et al.[44] Henan University of Science and Technology 20Cr2Ni4A When the mass fraction of Al is 0.007%, the coarsening temperature is
850 ℃; When the mass fraction of Al is 0.041%, the coarsening
temperature is 1030 ℃.Li et al.[45] Beijing University of Science and Technology L45 When mass fraction of Al ≥ 0.03%, the grain coarsening temperature can reach 1000 ℃ under the condition of long heating time. Kubota and Ochi[46] Nippon Steel Carburized anti-coarsening steel With the increase in Al addition, the grain coarsening temperature increases. However, when the amount of Al is too large, the grain coarsening temperature decreases. Sun et al.[47] Shouguang Juneng Special Steel 22CrMoH When the mass fraction of Al is low at 0.011%, less AlN will be formed, leading to the weakening of the pinning effect. The grain boundary will migrate at the position with less AlN, and the grains will grow. Qi and Li[37] Hebei Shigang 20MnCr5 When mass fraction of Al ≥ 0.025% and mass fraction ratio of Al/N≥3, no mixed crystal is formed at 930 ℃ for 6 h. Liu et al.[48] Beijing University of Science and Technology 20Cr When Nb is microalloyed and mass fraction of Al≥0.025%, the comprehensive pinning is the strongest. Li et al.[49] Fushun Special Steel 20MnCr5 When the mass fraction of Al ≥ 0.02% and mass fraction ratio of Al/N ≥ 2, the grain boundary can be effectively pinned to prevent grain growth and prolong the austenitization.
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State of Nb Mechanism Affecting stage Precipitated phase/
Solute (segregation)Pinning/Dragging
grain boundaryAustenitizing stage Precipitated phase/
Solute (segregation)Inhibit austenite recrystallization Recrystallization stage Precipitated phase Ferrite nucleation Solid-state transformation stage
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表 7 未溶解粒子的化學成分
Table 7. Chemical composition of undissolved particles
Element Mass fraction/% Atomic fraction/% C 4.96 25.40 Ti 14.03 18.02 V 3.98 4.81 Cr 1.53 1.80 Nb 75.49 49.97 Total 100 100
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表 8 Nb含量對奧氏體晶粒的影響
Table 8. Effect of Nb content on austenite grain
Author and publication Unit Steel Brief description Liu et al.[59] Central Iron & Steel
Research Institute0.065%C?1.15%Mn?0.055%Nb Steel When mass fraction of Nb ≤ 0.025%, no mixed structure appears. When mass fraction of Nb = 0.030%, a slightly mixed crystal structure appears. When mass fraction of Nb ≥ 0.035%, mixed crystals appear. The degree of mixed crystals increases with the Nb content. Yuan et al.[60] Northeast University C?Mn Steel With the increase in Nb content, the average size of austenite grains is refined from 248 nm to 69 nm, as shown in Figure 14. Kubota and Ochi[46] Nippon Steel Carburized anti-coarsening steel With the increase in Nb content, the grain coarsening temperature tends to increase. However, when the mass fraction of Nb exceeds 0.02%, the grain coarsening temperature does not increase further. Liu et al.[61] Kunming University of Science and Technology 17CrNiMo6 At a high temperature, the grain refining effect of AlN particles is not as significant as that of NbC particles. With the increase in Nb content, many undissolved NbC particles at high temperatures can play a strong role in inhibiting grain growth, as shown in Figure 15. Ma et al.[62] Central Iron & Steel
Research Institute20CrMoH The addition of Nb with a mass fraction of 0.04% can effectively refine grains, and the effect of controlling grain growth is not evident when the added mass fraction of Nb is 0 or 0.08%. Tong et al.[63] Shougang Group 20CrMnTi When the holding time is 1 h, the grain coarsening temperature increases by 50 ℃ for every 0.03% increase in mass fraction of Nb. Zhang et al.[57] Central Iron & Steel
Research Institute18Cr2Ni2Mo With the addition of Nb with a mass fraction of 0.01%, the gear steel becomes suitable for long-term carburization at 980 ℃, and the average grain size is about 26 μm. Jia et al.[64] Xining Special Steel 20MnCr5 After adding Nb with a mass fraction of 0.28%, the steel can meet the requirements of carburization at 1000 ℃ and no mixed crystal is formed.
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Table 9. Dissolution temperature formula and dissolution temperature of different precipitated particles[65?66]
Precipitated particle Dissolution temperature formula Starting solution temperature/℃ Complete solution temperature/℃ AlN $ \log [{\text{Al}}][{\text{N}}] = - \dfrac{{7550}}{T} + 1.93 $ 900–950 >1150 NbC $ \log [{\text{Nb}}][{\text{C}}] = - \dfrac{{7290}}{T} + 3.04 $ 950–1000 >1150 Nb(C, N) $ \log [{\text{Nb}}][{\text{C + N}}] = - \dfrac{{5860}}{T} + 1.54 $ >1050 >1300
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表 10 釘扎力模型的發展
Table 10. Development of pinning force model
Author and publication Unit Material Equation (Pz=) Brief description Smith[27] University of Chicago High purity aluminum $ \dfrac{{3\gamma f}}{{4r}} $ Original equation Gladman[26] United Steel $ \dfrac{{3\gamma f}}{{2r}} $ Only the particles behind the boundary affect the forward motion of the boundary, and the particles in front of the boundary increase the driving force. W?rner and Hazzledine[70] University of Valparaiso Electrical steel $ 1.38 \cdot \dfrac{{\gamma {f^{0.5}}}}{r} $ Influence of grain boundary migration mechanism on grains Nes et al.[29] Norwegian Institute of Technology $ 1.3 \cdot \dfrac{{\gamma {f^{0.92}}}}{r} $ When particles interact with the boundary, they produce a pinning effect and change the shape of the grain boundary. Wang et al.[71] Northeast University 20CrMoNb $ \dfrac{{6f\sigma }}{{\pi r}} $ Gladman equation, σ is the crystal plane energy Maalekian et al.[72] Columbia University Ti/Nb microalloyed Steel $ \beta \cdot \dfrac{{\gamma f}}{r} $ β is the grain boundary energy and an infinite constant determined by particle shape. Zhang et al.[73] Hokkaido University Hot rolled low alloy steel $ \dfrac{{3\gamma f}}{{2r}} $ Pinning force exerted by random particle distribution Gu et al.[74] Yanshan University X100 pipeline steel $ 12\gamma \displaystyle\sum\limits_i^{} {\dfrac{{{f_i}}}{{{r_i}}}} $
$ 12\gamma \displaystyle\sum\limits_{i = 0}^n {\dfrac{{{f_i}}}{{{r_i}}}} $A model with different types of particles (i represents all current precipitation phase types) Jiang et al.[75] Xining Special Steel Non-quenched and tempered steel $ \beta \cdot \dfrac{{\gamma f}}{r} $ Fine and dispersed MnS particles play a pinning role that can prevent grain growth. Liu et al.[76] Beijing University of Science and Technology 20Cr $ \beta \cdot \dfrac{{\gamma f}}{r} $ When $ f \geqslant 1.56 \times {10^{ - 4}} $,
abnormal grain growth can be avoided.Luo et al.[77] Kunming University of Science and Technology Ti-microalloyed steel $ \dfrac{{3\gamma fI}}{{2\pi {r^2}}} $ I is affected by $\displaystyle \sum\limits_{}^{} {f(r)} /r \cdot \displaystyle \sum\limits_0^n {f(r)} /r $
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表 11 加熱溫度對第二相粒子的影響
Table 11. Effect of heating temperature on second-phase particles
Author and publication Unit Steel Particle Brief description Yang et al.[78] Liaoning Special Steel FAS3220H-1 Nb(C, N) When the temperature exceeds 1000 ℃, grain growth is accelerated. Tong et al.[63] Shougang Group 20CrMnTiH NbC When the heating temperature is higher than 1000 ℃, some of the second-phase particles are dissolved. Meanwhile, the undissolved particles are coarsened. Liu et al.[79] Shougang Group 20CrMnTiH NbC, TiN High carburization temperature and time affect the coarsening of precipitated phase particles. Dong et al.[80] Shanghai Jiaotong University SA508-III AlN When the heating temperature is higher than 1050 ℃, grain coarsening occurs due to the dissolution of pinned particles.
Sun et al.[47] Shouguang Juneng Special Steel 22CrMoH AlN The coarsening temperature is 920–930 ℃. With the increase in temperature, AlN particles aggregates and dissolve, and the pinning effect weakens. Yang et al.[22] Angang 18CrNiMo7-6 NbC, AlN The optimal coarsening temperature is 1000 ℃.
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表 12 前人對混晶的研究結果
Table 12. Research results on mixed crystals in previous works
Author and publication Unit Steel Brief description Shen and Wu[82] Shougang Guiyang Special Steel 20CrMnTi The mixed crystal is caused by uneven temperature in the furnace and high local temperature, which results in abnormal coarse grains in the local part of the sample that form mixed crystals. Gao et al.[83] Luoyang Bearing Science & Technology Co., Ltd. Cr4Mo4V The uneven distribution of carbides easily occurs in metallurgical processes, and the mixed crystal structures are mainly caused by uneven primary carbides. Song[84] Hengye Forging F91 The alloying degree is relatively high, causing the structural heredity of the mixed crystal. During heat preservation, the increase in nonuniformity factor Z also increases the degree of crystal mixing. Liu et al.[85] Harbin Bearing Company 8Cr4Mo4V The mixed crystal structure after quenching is closely related to the grain size of raw materials. Ye et al.[86] Xining Special Steel 16MnCrS5＋H When mixed crystals appear after rolling, AlN can be fully precipitated after annealing at 760 ℃ in the two-phase zone, thus strengthening the role of AlN in pinning grains. Huang et al.[87] Anhui University of Technology 16MnCr5H The coarsening of austenite grains and the appearance of mixed grains are closely related to the aggregation and dissolution of the second-phase AlN particles.
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