鋯合金熱擠壓用防護潤滑劑的試制與性能

趙帆; 趙乙丞; 齊鵬; 張志豪

doi:10.13374/j.issn2095-9389.2020.01.15.001

鋯合金熱擠壓用防護潤滑劑的試制與性能

doi: 10.13374/j.issn2095-9389.2020.01.15.001

趙帆¹,
趙乙丞¹,
齊鵬²,
張志豪^1, ,

1.
北京科技大學新材料技術研究院，材料先進制備技術教育部重點實驗室，北京 100083
2.
國核寶鈦鋯業股份公司，寶雞 721013

基金項目: 國家重點研發計劃資助項目（2017YFB0306200）

詳細信息

通訊作者:
E-mail：ntzzh2279@163.com

中圖分類號: TG146.4⁺14
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出版歷程
- 收稿日期: 2020-01-15
- 刊出日期: 2021-02-26

Trial manufacture and properties of protective lubricants for hot extrusion of zirconium alloy

1.
Key Laboratory for Advanced Materials Processing (MOE), Institute for Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083, China
2.
State Nuclear Bao Ti Zirconium Industry Company, Baoji 721013, China

More Information

Corresponding author: E-mail: ntzzh2279@163.com

摘要

摘要: 為滿足鋯合金熱擠壓時的潤滑與防護需求，試制了一種鋯合金熱擠壓用防護潤滑劑，主要成分包括有機硅樹脂、低軟化點玻璃粉、氧化鋁粉、二硫化鉬、石墨粉、滑石粉、云母粉等。實驗溫度為700～800 ℃時，采用圓環壓縮法測得涂覆有潤滑劑的Zr-4合金摩擦因子為0.19～0.25，潤滑效果良好。將有潤滑劑防護的鋯合金分別加熱至700、800和900 ℃并保溫1 h，未發生明顯氧化，熱防護性能良好。測定了有、無潤滑劑條件下Zr-4合金和H13模具鋼的界面接觸溫度隨接觸時間的變化曲線。當Zr-4合金和H13鋼的初始界面溫度分別約為700 ℃和350 ℃時，無潤滑劑時Zr-4合金表面溫度達到穩定的時間為7.7 s，界面換熱系數由250 W·m^?2·℃^?1增大至2700 W·m^?2·℃^?1；有潤滑劑時Zr-4合金表面溫度達到穩定的時間延長至12 s，界面換熱系數由131 W·m^?2·℃^?1增大至1900 W·m^?2·℃^?1。這表明該潤滑劑具有較好的高溫熱障性能。
- 鋯合金 /
- 擠壓 /
- 潤滑劑 /
- 摩擦因子 /
- 熱防護
Abstract: Lubrication is the key in obtaining excellent products when zirconium alloys are hot extruded. Reasonable lubrication conditions are important to improve the product quality, reduce energy consumption, and prolong the service life of tools and dies. Presently, the glass lubricants commonly used in domestic industry are not very suitable for hot extrusion zirconium alloy, and they still need to be imported. In order to meet the requirements of lubrication and protection during hot extrusion of zirconium alloy, a protective lubricant for hot extrusion of zirconium alloy was trial manufactured in this paper. The main components of this protective lubricant include silicone resin, low softening point glass powder, aluminum oxide (Al₂O₃) powder, molybdenum disulfide, graphite powder, talcum powder, mica powder, and others. When the experimental temperature is in the range of 700?800 ℃, the friction factor of Zr-4 alloy coated with the lubricant is calculated to be 0.19?0.25 by the ring compression method, which shows good lubrication effect. The zirconium alloy with lubricant protection is not obviously oxidized after heating at 700 ℃, 800 ℃, and 900 ℃, respectively, for 1 h, indicating that the lubricant has good thermal protection effect. The relation curves between contact temperature and time at the interface of the Zr-4 alloy and H13 die steel are measured. The initial interface temperatures of the Zr-4 alloy and H13 steel are 700 ℃ and 350 ℃, respectively. Without the lubricant, the time for the surface temperature of the Zr-4 alloy to reach stability is 7.7 s, and the interfacial heat transfer coefficient increases from 250 W·m^?2·℃^?1 to 2700 W·m^?2·℃^?1. On the other and, when the lubricant was used, the time for the surface temperature of Zr-4 alloy to reach stability is prolonged to 12 s, and the interfacial heat transfer coefficient increases from 131 W·m^?2·℃^?1 to 1900 W·m^?2·℃^?1, indicating that the lubricant has good thermal barrier properties.
- zirconium alloy /
- extrusion /
- lubricant /
- friction factor /
- thermal protection

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圖 1 界面換熱實驗裝置示意圖

Figure 1. Schematic of interface heat exchange experimental device

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圖 2 加熱后的潤滑劑形貌。（a）配方1；（b）配方2

Figure 2. Morphology of the lubricant after heating: (a) formula 1; (b) formula 2

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圖 3 Zr-4合金試樣。（a）加熱前；（b）涂覆潤滑劑；（c）未涂覆潤滑劑

Figure 3. Zr-4 alloy sample: (a) before heating; (b) coated with lubricant; (c) uncoated with lubricant

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圖 4 Zr-4合金試樣橫截面形貌。（a）無潤滑劑，700 ℃；（b）無潤滑劑，800 ℃；（c）無潤滑劑，900 ℃；（d）有潤滑劑，700 ℃；（e）有潤滑劑，800 ℃；（f）有潤滑劑，900 ℃

Figure 4. Cross-sectional morphology of Zr-4 alloy: (a) without lubricant, 700 ℃; (b) without lubricant, 800 ℃; (c) without lubricant, 900 ℃; (d) with lubricant, 700 ℃; (e) with lubricant, 800 ℃; (f) with lubricant, 900 ℃

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圖 5 Zr-4合金與H13模具鋼換熱溫度?時間曲線。（a）有潤滑劑；（b）無潤滑劑

Figure 5. Temperature–time curves of heat exchange between the Zr-4 alloy and H13 die steel: (a) with lubricant; (b) without lubricant

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圖 6 Zr-4合金與H13模具鋼接觸面溫度變化與換熱系數

Figure 6. Heat transfer coefficient of contact surface of the Zr-4 alloy and H13 die steel

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表 1 無鉛低軟化點玻璃粉末主要成分（質量分數）

Table 1. Main components of lead-free low softening point glass powder %

P₂O₅	B₂O₃	ZnO	N₂O+K₂O
60	6	21	Bal.

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表 2 潤滑劑配方的質量比和狀態

Table 2. Mass ratio and status of lubricant formula

Formula	Glass powder	Silicone resin	Al₂O₃ power	Talcum powder	Mica powder	Status
1	6	2	1	1	1.5	Not soften; bubbles present
2	9	1	1	1	1.5	Poor adhesion
3	9	5	1	1	1.5	Carbonization
4	9	2	1	1	1.5	Good adhesion and fluidity

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表 3 添加不同含量二硫化鉬時的潤滑劑摩擦因子

Table 3. Friction factors of lubricants with different molybdenum disulfide contents

Mass fraction of MoS₂/%	Friction factors, m_t
5	0.48
10	0.34
20	0.31
30	0.29

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表 4 潤滑劑配方的質量比和摩擦因子

Table 4. Mass ratio and friction factors of lubricant formula

Formula	Glass powder	Silicone resin	Al₂O₃ power	Talcum powder	Mica powder	MoS₂ powder	Graphite powder	B₂O₃ powder	Friction factors, m_t
5	9	3	1.5	2	1	2	1.6	1.5	0.65
6	9	5	1.5	2	1	2	1.6	1.5
7	9	3	1.5	2	1	2	2	1
8	9	3	1.5	2	1	2	2	0	0.2

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表 5 潤滑劑基礎粉末成分（質量分數）

Table 5. Lubricant base powder composition %

Glass powder	Al₂O₃ power	Talcum powder	Mica powder	MoS₂	Graphite powder
50?60	5?10	10?15	5?10	10?15	10?15

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表 6 圓環壓縮實驗結果

Table 6. Results of ring compression experiments

Sample	Lubricant	Temperature / ℃	Friction factors, m_t
1	No lubricant	750	1
2	Westinghouse	700	0.20±0.01
3	Westinghouse	750	0.22±0.02
4	Westinghouse	800	0.27±0.01
7	Present study	700	0.19±0.01
8	Present study	750	0.20±0.01
9	Present study	800	0.25±0.01

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259luxu-164

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