CN105401083A - Sealing alloy for moderate-high-temperature evacuated solar collector tubes, preparation method for sealing alloy and using method of sealing alloy - Google Patents
Sealing alloy for moderate-high-temperature evacuated solar collector tubes, preparation method for sealing alloy and using method of sealing alloy Download PDFInfo
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Abstract
The invention discloses sealing alloy for moderate-high-temperature evacuated solar collector tubes, a preparation method for the sealing alloy and a using method of the sealing alloy, and belongs to the technical field of photo-thermal utilization of solar energy. The sealing alloy is prepared through material preparation, smelting, casting and thermal treatment. The prepared sealing alloy is machined into a workpiece of the needed size and in the needed shape, the surface of the workpiece is sequentially subjected to oil and grease removal cleaning, sand blasting and hydrogen burning or vacuum degassing treatment, and then sealing of the workpiece and glass can be conducted. The sealing alloy is superior in working performance, good in glass matching performance and wide in working temperature range. The preparation process for the sealing alloy is simple and easy to operate. The sealing alloy is suitable for the moderate-high-temperature evacuated solar collector tubes or other fields with special requirements for the coefficient of thermal expansion.
Description
Technical field
The invention belongs to solar energy thermal utilization technical field, particularly the effective sealing alloy of middle high temperature solar vacuum heat-collecting and preparation and application thereof.
Background technology
Middle high temperature solar vacuum heat collection pipe is the key part of solar energy light gathering and heat collecting generating, its corrugated tube preparing pipe, glass enclosure tube and two ends compensate for dilatation amount difference in the stainless steel of heat absorbing coating by surface forms, and forms vacuum annular space in stainless steel between pipe and glass enclosure tube.The vacuum tightness of vacuum annular space on the impact of thermal-collecting tube collecting efficiency greatly.For meeting the vacuum requirement of thermal-collecting tube, reducing thermosteresis, improving collecting efficiency, must ensure to be tightly connected between pipe in glass enclosure tube and stainless steel, and the cold cycling operating mode (being generally 25-550 DEG C) when solar energy heat collection pipe runs can be adapted to.Therefore, to need in glass enclosure tube and stainless steel between pipe, to introduce the sealing alloy matched with thermal expansion coefficient of glass, avoid glass/metal thermal expansivity in thermal-collecting tube operational process not mate and the destruction of causing.
Sealing alloy conventional at present has 4J29, Ni-Co (ZL90102845) etc.But above-mentioned alloy working temperature low (about 25-450 DEG C), be difficult to the requirement meeting high temperature solar vacuum heat collection pipe, therefore, mate well with glass in the urgent need to a kind of working temperature high (25-550 DEG C), thermal expansivity, be easy to weld, be easy to the novel glass metal sealing alloy prepared, with the demand of high temperature solar thermal utilization large size valve tube in meeting.
Summary of the invention
The present invention is directed to the shortcoming of prior art, provide the effective sealing alloy of high temperature solar vacuum heat-collecting and preparation and application thereof in one.
To achieve these goals, the technical scheme taked of the present invention is as follows:
The effective sealing alloy of high temperature solar vacuum heat-collecting in one, described sealing alloy is made up of the component of following parts by weight: iron 40-60 part, nickel 25-45 part, and other metals are 0-25 part, and rare earth metal is 2-5 part;
Other described metals are one or more in B, V, Cr, Mn, Co, Cu, Mo, Nb and Y; Described rare earth metal is one or more in La, Ce and Yb.
In described sealing alloy, the parts by weight of iron are preferably 40-50 part.
The starting material of described sealing alloy component are followed successively by: pure metal iron, pure metallic nickel, other metals or its alloy, rare earth metal or its alloy.
The purity of described pure metal iron and pure metallic nickel is more than 99.5%.
Described sealing alloy operating temperature range is 25-550 DEG C, and in operating temperature range, its thermal expansivity and the coefficient of expansion are 2.7 × 10
-6-5.5 × 10
-6the glassy phase coupling of 1/K.
The preparation method of the described effective sealing alloy of a kind of middle high temperature solar vacuum heat-collecting, comprises the following steps:
(1) get the raw materials ready: according to the weight of each component of sealing alloy, take starting material; Starting material after cleaning process, then carry out bakeout degassing, obtain pretreated starting material;
(2) melting: adopt vacuum arc fumace or vacuum medium frequency induction furnace to carry out melting to pretreated starting material, after it melts completely, then continue refining 10-30 minute;
(3) pour into a mould: adopt the cast of the method for suction pouring or the starting material after refining are cast in water cooled mo(u)ld, making its rapid solidification obtain ingot casting; Described teeming temperature is 1470-1520 DEG C;
(4) thermal treatment: the ingot casting obtained is heat-treated under inert atmosphere protection, process of thermal treatment is: 1100-1300 DEG C, insulation 1-2 hour, ensures ingot casting high temperature solid solution body phase region uniform composition; Be cooled to 850-950 DEG C, insulation 3-6 hour, ensure that ingot casting all changes middle temperature solid solution phase into, and uniform composition; Finally be cooled to room temperature, obtain sealing alloy.
The time of described bakeout degassing is more than 1 hour.
The described method taked that cools rapidly is oil quenching or shrend.
Described rare gas element is nitrogen or argon gas.
The using method of the effective sealing alloy of described middle high temperature solar vacuum heat-collecting is: the machined workpiece for desired size and shape of sealing alloy, workpiece surface is after oil removing, degrease cleaning, surface sand-blasting, then carry out annealing in hydrogen atmosphere or vacuum stripping process, sealing-in can be carried out with glass.
Beneficial effect of the present invention is: the sealing alloy serviceability of preparation is excellent, good with glass matched performance; Operating temperature range is wide, higher than the working temperature of common sealing alloy about 100 DEG C, and its manufacturing process is simple, easy to operate.Sealing alloy prepared by the present invention can be prepared into band and the ring of various shape, is applicable to middle high temperature solar vacuum heat collection pipe or other has the field of specific demand to thermal expansivity.
Accompanying drawing explanation
The moiety weight range figure (region that some a → b → c → d → e → f → a surrounds) that Fig. 1 is the effective sealing alloy of middle high temperature solar vacuum heat-collecting; Wherein, M represents the weight range of other metals and rare earth metal, wt.% (M)=wt.% (other metal)+wt.% (rare earth metal).
Fig. 2 is the hot expansibility graphic representation of Fe-35wt.%Ni-8wt.%Co-2wt.%Cu-2wt.%Y-3wt.%Ce sealing alloy.
Fig. 3 is the hot expansibility graphic representation of Fe-25wt.%Ni-4wt.%Mn-11wt.%Co-5wt.%Ce sealing alloy.
Fig. 4 is the hot expansibility graphic representation of Fe-30wt.%Ni-18wt.%Co-5wt.%Mo-2wt.%V-5wt.%Ce sealing alloy.
Fig. 5 is the hot expansibility graphic representation of Fe-45wt.%Ni-4wt.%Cr-6wt.%Mn-2wt.%V-2wt.%Ce-1wt.%La sealing alloy.
Fig. 6 is the hot expansibility graphic representation of Fe-45wt.%Ni-1wt.%Co-2wt.%La sealing alloy.
Fig. 7 is the hot expansibility graphic representation of Fe-40wt.%Ni-1wt.%Co-2wt.%Ce sealing alloy.
Fig. 8 is the hot expansibility curve of Fe-25wt.%Ni-7.4wt.%Co-4.4wt.%B-3.2wt.%Ce sealing alloy.
Embodiment
Embodiment 1:
(1) starting material adopt pure Fe (purity >=99.5%), Ni (purity >=99.5%), Co (purity >=99.4%), Cu (purity >=99.4%), Y (purity is greater than 99.5%), Ce (purity >=99.0%).Sealing alloy moiety proportioning, with the proportions of Fig. 1 g point, the proportioning shown in embodiment 1 namely in table 1: Fe-35wt.%Ni-8wt.%Co-2wt.%Cu-2wt.%Y-3wt.%Ce.
(2) according to said ratio, starting material are taken; After starting material oil removing, degrease, washing cleaning, be placed in crucible bakeout degassing 2 hours, obtain pretreated starting material;
(3) vacuum arc fumace is adopted to carry out melting to pretreated starting material; When smelting temperature reaches 1400-1500 DEG C, starting material start fusing; After it melts completely, then continue refining 20 minutes;
(4) adopt the method for suction pouring to pour into a mould the starting material after refining, make its rapid solidification obtain ingot casting, teeming temperature is 1470-1520 DEG C;
(5) ingot casting is heat-treated under nitrogen, argon gas atmosphere protection, and process of thermal treatment is: 1200 DEG C, is incubated 1 hour; Be cooled to 900 DEG C again, be incubated 4 hours; Be cooled to room temperature rapidly finally by employing oil quenching, obtain sealing alloy.
(6) spillikin sealing alloy obtained being cut into Φ 4 × 25mm carries out hot expansibility test test; Temperature rise rate is 5 DEG C/min, Range of measuring temp be room temperature to 650 DEG C, test result is as shown in Figure 2.
Embodiment 2:
(1) raw material adopts pure Fe (purity >=99.5%), Ni (purity >=99.5%), Co (purity >=99.4%), Mn (purity >=99.4%), Ce (purity >=99.0%).Sealing alloy moiety proportioning, with the proportions of Fig. 1 a point, the proportioning shown in embodiment 2 namely in table 1: Fe-25wt.%Ni-4wt.%Mn-11wt.%Co-5wt.%Ce;
(2) according to said ratio, starting material are taken; After starting material oil removing, degrease, washing cleaning, be placed in crucible bakeout degassing 1 hour, obtain pretreated starting material;
(3) vacuum medium frequency induction furnace is adopted to carry out melting to pretreated starting material; When smelting temperature reaches 1400-1500 DEG C, starting material start fusing; After it melts completely, then continue refining 15 minutes;
(4) be poured in water cooled mo(u)ld by the starting material after refining and make its rapid solidification obtain ingot casting, teeming temperature is 1470-1520 DEG C;
(5) ingot casting is heat-treated under nitrogen, argon gas atmosphere protection, and process of thermal treatment is: 1100 DEG C, is incubated 2 hours; Be cooled to 850 DEG C again, be incubated 5 hours; Be cooled to room temperature rapidly finally by employing oil quenching, obtain sealing alloy.
(6) spillikin sealing alloy obtained being cut into Φ 4 × 25mm carries out hot expansibility test test; Temperature rise rate is 5 DEG C/min, Range of measuring temp be room temperature to 650 DEG C, test result is as shown in Figure 3.
Embodiment 3
(1) raw material adopts pure Fe (purity >=99.5%), Ni (purity >=99.5%), Co (purity >=99.4%), V (purity is greater than 99.5%), Ce (purity >=99.0%).Sealing alloy moiety proportioning, with the proportions of Fig. 1 b point, the proportioning shown in embodiment 3 namely in table 1: Fe-30wt.%Ni-18wt.%Co-5wt.%Mo-2wt.%V-5wt.%Ce;
(2) according to said ratio, starting material are taken; After starting material oil removing, degrease, washing cleaning, be placed in crucible bakeout degassing 1.5 hours, obtain pretreated starting material;
(3) vacuum medium frequency induction furnace is adopted to carry out melting to pretreated starting material; When smelting temperature reaches 1400-1500 DEG C, starting material start fusing; After it melts completely, then continue refining 30 minutes;
(4) be poured in water cooled mo(u)ld by the starting material after refining and make its rapid solidification obtain ingot casting, teeming temperature is 1470-1520 DEG C;
(5) ingot casting is heat-treated under nitrogen, argon gas atmosphere protection, and process of thermal treatment is: 1300 DEG C, is incubated 1 hour; Be cooled to 950 DEG C again, be incubated 3 hours; Be cooled to room temperature rapidly finally by employing shrend, obtain sealing alloy.
(6) spillikin sealing alloy obtained being cut into Φ 4 × 25mm carries out hot expansibility test test; Temperature rise rate is 5 DEG C/min, Range of measuring temp be room temperature to 650 DEG C, test result is as shown in Figure 4.
Embodiment 4
(1) raw material adopts pure Fe (purity >=99.5%), Ni (purity >=99.5%), Cr (purity >=99.4%), Mn (purity >=99.4%), V (purity is greater than 99.5%), Ce (purity >=99.0%), La (purity >=99.0%).Sealing alloy moiety proportioning, with the proportions of Fig. 1 c point, the proportioning shown in embodiment 4 namely in table 1: Fe-45wt.%Ni-4wt.%Cr-6wt.%Mn-2wt.%V-2wt.%Ce-1wt.%La;
(2) according to said ratio, starting material are taken; After starting material oil removing, degrease, washing cleaning, be placed in crucible bakeout degassing 1 hour, obtain pretreated starting material;
(3) vacuum medium frequency induction furnace is adopted to carry out melting to pretreated starting material; When smelting temperature reaches 1400-1500 DEG C, starting material start fusing; After it melts completely, then continue refining 25 minutes;
(4) be poured in water cooled mo(u)ld by the starting material after refining and make its rapid solidification obtain ingot casting, teeming temperature is 1470-1520 DEG C;
(5) ingot casting is heat-treated under nitrogen, argon gas atmosphere protection, and process of thermal treatment is: 1200 DEG C, is incubated 1.5 hours; Be cooled to 900 DEG C again, be incubated 5 hours; Be cooled to room temperature rapidly finally by employing shrend, obtain sealing alloy.
(6) spillikin sealing alloy obtained being cut into Φ 4 × 25mm carries out hot expansibility test test; Temperature rise rate is 5 DEG C/min, Range of measuring temp be room temperature to 650 DEG C, test result is as shown in Figure 5.
Embodiment 5:
(1) raw material adopts pure Fe (purity >=99.5%), Ni (purity >=99.5%), Co (purity >=99.4%), Cu (purity >=99.4%), La (purity >=99.0%).Sealing alloy moiety proportioning, with the proportions of Fig. 1 d point, the proportioning shown in embodiment 5 namely in table 1: Fe-45wt.%Ni-1wt.%Co-2wt.%La;
(2) according to said ratio, starting material are taken; After starting material oil removing, degrease, washing cleaning, be placed in crucible bakeout degassing 2 hours, obtain pretreated starting material;
(3) vacuum medium frequency induction furnace is adopted to carry out melting to pretreated starting material; When smelting temperature reaches 1400-1500 DEG C, starting material start fusing; After it melts completely, then continue refining 10 minutes;
(4) adopt the method for suction pouring to pour into a mould the starting material after refining, make its rapid solidification obtain ingot casting, teeming temperature is 1470-1520 DEG C;
(5) ingot casting is heat-treated under nitrogen, argon gas atmosphere protection, and process of thermal treatment is: 1200 DEG C, is incubated 1.5 hours; Be cooled to 900 DEG C again, be incubated 5 hours; Be cooled to room temperature rapidly finally by employing shrend, obtain sealing alloy.
(6) spillikin sealing alloy obtained being cut into Φ 4 × 25mm carries out hot expansibility test test; Temperature rise rate is 5 DEG C/min, Range of measuring temp be room temperature to 650 DEG C, test result is as shown in Figure 6.
Embodiment 6
(1) raw material adopts pure Fe (purity >=99.5%), Ni (purity >=99.5%), Co (purity >=99.4%), Ce (purity >=99.0%).Sealing alloy moiety proportioning, with the proportions of Fig. 1 e point, the proportioning shown in embodiment 6 namely in table 1: Fe-40wt.%Ni-1wt.%Co-2wt.%Ce;
(2) according to said ratio, starting material are taken; After starting material oil removing, degrease, washing cleaning, be placed in crucible bakeout degassing 2 hours, obtain pretreated starting material;
(3) vacuum medium frequency induction furnace is adopted to carry out melting to pretreated starting material; When smelting temperature reaches 1400-1500 DEG C, starting material start fusing; After it melts completely, then continue refining 30 minutes;
(4) be poured in water cooled mo(u)ld by the starting material after refining and make its rapid solidification obtain ingot casting, teeming temperature is 1470-1520 DEG C;
(5) ingot casting is heat-treated under nitrogen, argon gas atmosphere protection, and process of thermal treatment is: 1300 DEG C, is incubated 1 hour; Be cooled to 850 DEG C again, be incubated 6 hours; Be cooled to room temperature rapidly finally by employing oil quenching, obtain sealing alloy.
(6) spillikin sealing alloy obtained being cut into Φ 4 × 25mm carries out hot expansibility test test; Temperature rise rate is 5 DEG C/min, Range of measuring temp be room temperature to 650 DEG C, test result is as shown in Figure 7.
Embodiment 7
(1) raw material adopts pure Fe (purity >=99.5%), Ni (purity >=99.5%), Co (purity >=99.4%), B (purity >=99.4%), Ce (purity >=99.0%).Sealing alloy moiety proportioning, with the proportions of Fig. 1 f point, the proportioning shown in embodiment 7 namely in table 1: Fe-25wt.%Ni-7.4wt.%Co-4.4wt.%B-3.2wt.%Ce;
(2) according to said ratio, starting material are taken; After starting material oil removing, degrease, washing cleaning, be placed in crucible bakeout degassing 1 hour, obtain pretreated starting material;
(3) vacuum medium frequency induction furnace is adopted to carry out melting to pretreated starting material; When smelting temperature reaches 1400-1500 DEG C, starting material start fusing; After it melts completely, then continue refining 10 minutes;
(4) adopt the method for suction pouring to pour into a mould the starting material after refining, make its rapid solidification obtain ingot casting, teeming temperature is 1470-1520 DEG C;
(5) ingot casting is heat-treated under nitrogen, argon gas atmosphere protection, and process of thermal treatment is: 1300 DEG C, is incubated 1 hour; Be cooled to 950 DEG C again, be incubated 3 hours; Be cooled to room temperature rapidly finally by employing oil quenching, obtain sealing alloy.
(6) spillikin sealing alloy obtained being cut into Φ 4 × 25mm carries out hot expansibility test test; Temperature rise rate is 5 DEG C/min, Range of measuring temp be room temperature to 650 DEG C, test result is as shown in Figure 8.
Table 1 embodiment 1-7 sealing alloy moiety proportioning
The hot expansibility test result of gained sealing alloy as illustrated in figs. 2 through 8.As we know from the figure, the working temperature of gained sealing alloy material is high, and in wide temperature range, (25-550 DEG C) thermal expansivity can be 2.7 × 10 with the coefficient of expansion
-6-5.5 × 10
-6the glassy phase coupling of 1/K.
Claims (10)
1. in, the effective sealing alloy of high temperature solar vacuum heat-collecting, is characterized in that, described alloy is made up of the component of following parts by weight: iron 40-60 part, nickel 25-45 part, and other metals are 0-25 part, and rare earth metal is 2-5 part;
Wherein, other described metals are one or more in B, V, Cr, Mn, Co, Cu, Mo, Nb and Y; Described rare earth metal is one or more in La, Ce and Yb.
2. the effective sealing alloy of high temperature solar vacuum heat-collecting in one according to claim 1, is characterized in that, in described sealing alloy, the parts by weight of iron are preferably 40-50 part.
3. the effective sealing alloy of high temperature solar vacuum heat-collecting in one according to claim 1, is characterized in that, the starting material of described sealing alloy component are followed successively by: pure metal iron, pure metallic nickel, other metals or its alloy, rare earth metal or its alloy.
4. the effective sealing alloy of high temperature solar vacuum heat-collecting in one according to claim 3, is characterized in that, the purity of described pure metal iron and pure metallic nickel is more than 99.5%.
5. the effective sealing alloy of high temperature solar vacuum heat-collecting in one according to claim 1, is characterized in that, described sealing alloy operating temperature range is 25-550 DEG C, and in operating temperature range, its thermal expansivity and the coefficient of expansion are 2.7 × 10
-6-5.5 × 10
-6the glassy phase coupling of 1/K.
6. the preparation method of the effective sealing alloy of middle high temperature solar vacuum heat-collecting described in any one of claim 1-5, comprises the following steps:
(1) get the raw materials ready: according to the weight proportion of each component of sealing alloy, take starting material; Starting material after cleaning process, then carry out bakeout degassing, obtain pretreated starting material;
(2) melting: adopt vacuum arc fumace or vacuum medium frequency induction furnace to carry out melting to pretreated starting material, after it melts completely, then refining 10-30 minute;
(3) pour into a mould: adopt the cast of the method for suction pouring or the starting material after refining are cast in water cooled mo(u)ld, making its rapid solidification obtain ingot casting; Described teeming temperature is 1470-1520 DEG C;
(4) thermal treatment: the ingot casting obtained is heat-treated under inert atmosphere protection, process of thermal treatment is: 1100-1300 DEG C, insulation 1-2 hour; Be cooled to 850-950 DEG C, insulation 3-6 hour; Finally be cooled to room temperature rapidly, obtain sealing alloy.
7. the preparation method of the effective genus sealing alloy of a kind of middle high temperature solar vacuum heat-collecting according to claim 6, it is characterized in that, the time of described bakeout degassing is more than 1 hour.
8. the preparation method of the effective sealing alloy of a kind of middle high temperature solar vacuum heat-collecting according to claim 6, is characterized in that, the described method taked that cools rapidly is oil quenching or shrend.
9. the preparation method of the effective sealing alloy of a kind of middle high temperature solar vacuum heat-collecting according to claim 6, is characterized in that, described rare gas element is nitrogen or argon gas.
10. the using method of the effective sealing alloy of a kind of middle high temperature solar vacuum heat-collecting described in any one of claim 1-5 is: the machined workpiece for desired size and shape of sealing alloy, workpiece surface is after oil removing, degrease cleaning, surface sand-blasting, carry out annealing in hydrogen atmosphere or vacuum stripping process again, sealing-in can be carried out with glass.
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2015
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US3954509A (en) * | 1974-05-02 | 1976-05-04 | The International Nickel Company, Inc. | Method of producing low expansion alloys |
JPS5651555A (en) * | 1979-10-03 | 1981-05-09 | Toshiba Corp | Dumet wire |
CN87101657A (en) * | 1987-03-05 | 1988-11-30 | 清华大学 | Seal alloy of resistance to silver soldering brittleness |
CN1200409A (en) * | 1997-05-23 | 1998-12-02 | 陕西钢铁研究所 | Low cobalt enamel sealed iron-nickel-cobalt alloy |
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