CN103374670A - Lead-stibium-rare earth alloy adhesive and preparation method thereof - Google Patents
Lead-stibium-rare earth alloy adhesive and preparation method thereof Download PDFInfo
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- CN103374670A CN103374670A CN2013102799194A CN201310279919A CN103374670A CN 103374670 A CN103374670 A CN 103374670A CN 2013102799194 A CN2013102799194 A CN 2013102799194A CN 201310279919 A CN201310279919 A CN 201310279919A CN 103374670 A CN103374670 A CN 103374670A
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Abstract
The invention relates to a lead-stibium-rare earth alloy adhesive comprising the following components in percentage by weight: 87.0-92.0% of lead, 7.0-12.0% of stibium, 0.1-0.5% of arsenium, 0.1-0.5% of lanthanum and 0.0-0.25% of cerium, wherein the alloy adhesive with the formula contains less than 0.5% of impurities including aluminum, silicon and ferrum. When the lead-stibium-rare earth alloy adhesive is prepared, firstly, a lead-rare earth alloy intermediate is prepared, stibium and arsenium are added in the molten lead, and the lead-rare earth alloy intermediate is added when the melting is completed. The technical method disclosed by the invention is simple and convenient in operation; and the prepared alloy adhesive can have stronger harmful stress resistance and can be better combined with porcelain and metal ware so that the porcelain is prevented from being damaged.
Description
Technical field
The present invention relates to a kind of alloy encapsulated material for insulator, can be suitable for specifically a kind of alloy cementing agent that contains rare metal of extreme environment, belong to field of alloy material.
Background technology
Along with the development of power industry, ultra-high voltage, large span, long distance power transmission have obtained popularizing rapidly, and abominable physical environment has proposed higher specification of quality to the insulator product.Wherein, cementing agent plays integrally-built tissue-welding effect, and its quality is directly connected to the performance of insulator, life-span and reliability.The present high-quality insulator cementing agent of insulator product significant need especially can be applicable to the alloy cementing agent of extreme natural environment.
The someone attempts lead antimony alloy as the insulator cementing agent at present.200510041232.2) and " a kind of alloy cementing agent is filled a prescription and its preparation method and application " (application number: 201210265774.8) patent " electric transmission and distribution circuit insulator with cementing agent lead antimony alloy and preparation method thereof " (application number: for example.The alloy cementing agent of aforesaid method preparation satisfies the insulator industry for a part of demand of high quality alloy cementing agent, and 20～100 ℃ thermal expansivity of its preparation alloy cementing agent is (18～28) * 10
-6K
-1, still have with the thermal expansivity of High-Alumina pottery and used metal-ware thereof that (thermal expansivity of High-Alumina pottery is about 4.1 * 10 than big difference
-6K
-1, the thermal expansivity of metal-ware is about 1.2 * 10
-6K
-1).When insulator environment for use temperature variation is larger, if use above-mentioned alloy cementing agent, when variation of ambient temperature is larger, still can produce no small internal stress, have the hidden danger of insulator infringement.
Summary of the invention
For solving the deficiencies in the prior art, the object of the present invention is to provide a kind of alloy cementing agent prescription with less thermal expansion coefficient difference and its preparation method and application.
For achieving the above object, the present invention is achieved by the following technical solutions:
A kind of plumbous antimony rare earth alloy cementing agent, its prescription comprises that the weight percent of following component and each component is:
The preparation method of above-mentioned plumbous antimony rare earth alloy cementing agent may further comprise the steps:
(1) get the raw materials ready: the prescription according to above-mentioned plumbous antimony rare earth alloy cementing agent is prepared metallic lead, antimony, arsenic and rare metal lanthanum cerium;
(2) baker: crucible temperature is set as 200 ℃, adds a small amount of charcoal and carry out baker, furnace drying time is 0.8～1h, keeps the crucible inner drying, without other impurity;
(3) preparation plumbum rare earth alloy intermediate: when furnace temperature reaches 200 ℃, add lead, continue to be heated to 350～400 ℃, stopped heating insulation 10～15 minutes; Continue to be warming up to 920 ℃; Add the rare earth lanthanum cerium, drag for slag after continuing stirring and being incubated 20 minutes; Then cool to room temperature.
(4) preparation alloy cementing agent: dry boiler is heated to 200 ℃, then to wherein adding lead, antimony and arsenic, in dry boiler, adds wood charcoal powder simultaneously, then be heated to 550～600 ℃, remain that wood charcoal powder covers liquid level; Under this temperature, be incubated and stirred 2～5 minutes, form uniform plumbous antimony arsenic liquation; Add the plumbum rare earth alloy intermediate, all after the fusing, after insulation under this temperature and stirring 30～40 minutes, 1～5% the paraffin that adds plumbous antimony rare earth alloy total mass, then the rear slagging-off that stirs is incubated 15～20min and obtains the alloy cementing agent, then carries out insulator cementing.
Lead described in the step (1) and the particle diameter of antimony are 10～20mm, and the particle diameter of arsenic, lanthanum and cerium is 1～2mm.
In the process of step (3) preparation plumbum rare earth alloy intermediate, lead requires at 50:1～20:1 with lanthanum and cerium quality adding proportion, and the per-cent that cerium accounts for lanthanum cerium quality is not more than 50%.
50～100 ℃/h of all heat-up rate controls in step (2), step (3) and the step (4).
It is 2min that stirring insulating process in step (3) and the step (4) requires the mixing chamber interval, and each churning time is 2～3min.
Alloy cementing agent of the present invention is applied in the insulator cementing.
The invention has the beneficial effects as follows: the alloy cementing agent that the present invention is prepared, by reasonable interpolation rare metal lanthanum, the perhaps combination of lanthanum and cerium makes the crystal grain of alloy become tiny even, can improve the comprehensive mechanical property of alloy, falls to make its more flexible; Low-alloyed thermal expansivity can fall, connection porcelain piece and metal-ware that it is more closed.
Embodiment
Below in conjunction with specific embodiment the present invention is done concrete introduction.
Embodiment 1: a kind of plumbous antimony rare earth alloy cementing agent, and the weight percent of its recipe ingredient and each component is:
Wherein, the content of impurity aluminum, silicon, iron was less than 0.5% during the alloy cementing agent was filled a prescription.
The preparation method of above-mentioned plumbous antimony rare earth alloy cementing agent may further comprise the steps:
(1) gets the raw materials ready: prepare metallic lead, antimony, arsenic and rare metal lanthanum, cerium; Allot the alloy cementing agent of 2Kg according to the prescription of above-mentioned plumbous antimony rare earth alloy cementing agent,
(2) baker: crucible temperature is set as 200 ℃, adds a small amount of charcoal and carry out baker, furnace drying time is 1h, keeps the crucible inner drying, without other impurity;
(3) preparation plumbum rare earth alloy intermediate: when furnace temperature reaches 200 ℃, add plumbous 400g, continue to be heated to 380 ℃, stopped heating insulation 10 minutes; Continue to be warming up to 920 ℃; Add 6g lanthanum and 2g cerium, drag for slag after continuing stirring and being incubated 20 minutes; Then cool to room temperature.
(4) preparation alloy cementing agent: dry boiler is heated to 200 ℃, then to wherein adding plumbous 1390g, antimony 194g and arsenic 8g, in dry boiler, adds wood charcoal powder simultaneously, then be heated to 600 ℃, remain that wood charcoal powder covers liquid level; Under this temperature, be incubated and stirred 3 minutes, form uniform plumbous antimony arsenic liquation; Add the plumbum rare earth alloy intermediate, all after the fusing, after insulation under this temperature and stirring 40 minutes, add 3.0% paraffin of plumbous antimony rare earth alloy total mass, then the rear slagging-off that stirs is incubated 15min and obtains the alloy cementing agent, then carries out insulator cementing.Stay a part of alloy sample calorimetric coefficient of expansion.
Particle diameter plumbous and antimony is 10～20mm, and the particle diameter of arsenic, lanthanum and cerium is 1～2mm; 50 ℃/h of all heat-up rate controls in the preparation process; Alr mode is to be pitch time 2min, and each churning time is 3min.
Instrument specification and producer are as follows:
The Shanghai special one-tenth mechanical means SG2-3-10 of company limited crucible oven;
Xiang Tan China elegant demeanour device PCY of Manufacturing Co., Ltd type high-temperature horizontal dilatometer.
Material choice producer and purity are as follows:
Embodiment 2: substantially the same manner as Example 1, difference is the proportioning raw materials of plumbous antimony rare earth alloy cementing agent: lead 87.0%, antimony 12.0%, arsenic 0.5%, lanthanum 0.5%.
The preparation method of above-mentioned plumbous antimony rare earth alloy cementing agent may further comprise the steps:
(1) gets the raw materials ready: prepare metallic lead, antimony, arsenic and rare metal lanthanum; Allot the alloy cementing agent of 2Kg according to the prescription of above-mentioned plumbous antimony rare earth alloy cementing agent,
(2) baker: crucible temperature is set as 200 ℃, adds a small amount of charcoal and carry out baker, furnace drying time is 1h, keeps the crucible inner drying, without other impurity;
(3) preparation plumbum rare earth alloy intermediate: when furnace temperature reaches 200 ℃, add plumbous 400g, continue to be heated to 350～400 ℃, stopped heating insulation 12 minutes; Continue to be warming up to 920 ℃; Add the 10g lanthanum, drag for slag after continuing stirring and being incubated 20 minutes; Then cool to room temperature.
(4) preparation alloy cementing agent: dry boiler is heated to 200 ℃, then to the antimony and the arsenic that wherein add in remaining lead and the prescription, in dry boiler, adds wood charcoal powder simultaneously, then be heated to 550 ℃, remain that wood charcoal powder covers liquid level; Under this temperature, be incubated and stirred 2 minutes, form uniform plumbous antimony arsenic liquation; Add the plumbum rare earth alloy intermediate, all after the fusing, after insulation under this temperature and stirring 40 minutes, add 1% paraffin of plumbous antimony rare earth alloy total mass, then the rear slagging-off that stirs is incubated 15min and obtains the alloy cementing agent, then carries out insulator cementing.Stay a part of alloy sample calorimetric coefficient of expansion.
Particle diameter plumbous and antimony is 10～20mm, and the particle diameter of arsenic, lanthanum and cerium is 1～2mm; 70 ℃/h of all heat-up rate controls in the preparation process; Alr mode is to be pitch time 2min, and each churning time is 2min.
Embodiment 3: substantially the same manner as Example 1, difference is the proportioning raw materials of plumbous antimony rare earth alloy cementing agent: lead 92.0%, antimony 7.0%, arsenic 0.5%, lanthanum 0.4% and cerium 0.1%.
The preparation method of above-mentioned plumbous antimony rare earth alloy cementing agent may further comprise the steps:
(1) gets the raw materials ready: prepare metallic lead, antimony, arsenic and rare metal lanthanum, cerium; Allot the alloy cementing agent of 2Kg according to the prescription of above-mentioned plumbous antimony rare earth alloy cementing agent,
(2) baker: crucible temperature is set as 200 ℃, adds a small amount of charcoal and carry out baker, furnace drying time is 1h, keeps the crucible inner drying, without other impurity;
(3) preparation plumbum rare earth alloy intermediate: when furnace temperature reaches 200 ℃, add plumbous 300g, continue to be heated to 400 ℃, stopped heating insulation 15 minutes; Continue to be warming up to 920 ℃; Add 8g lanthanum and 2g cerium, drag for slag after continuing stirring and being incubated 20 minutes; Then cool to room temperature.
(4) preparation alloy cementing agent: dry boiler is heated to 200 ℃, then to the antimony and the arsenic that wherein add in remaining lead and the prescription, in dry boiler, adds wood charcoal powder simultaneously, then be heated to 580 ℃, remain that wood charcoal powder covers liquid level; Under this temperature, be incubated and stirred 5 minutes, form uniform plumbous antimony arsenic liquation; Add the plumbum rare earth alloy intermediate, all after the fusing, after insulation under this temperature and stirring 40 minutes, add 2% paraffin of plumbous antimony rare earth alloy total mass, then the rear slagging-off that stirs is incubated 15min and obtains the alloy cementing agent, then carries out insulator cementing.Stay a part of alloy sample calorimetric coefficient of expansion.
Particle diameter plumbous and antimony is 10～20mm, and the particle diameter of arsenic, lanthanum and cerium is 1～2mm; 100 ℃/h of all heat-up rate controls in the preparation process; Alr mode is to be pitch time 2min, and each churning time is 3min.
Embodiment 4: substantially the same manner as Example 1, difference is the proportioning raw materials of plumbous antimony rare earth alloy cementing agent: lead 89%, antimony 10.5%, arsenic 0.1%, lanthanum 0.3% and cerium 0.1%.
The preparation method of above-mentioned plumbous antimony rare earth alloy cementing agent may further comprise the steps:
(1) gets the raw materials ready: prepare metallic lead, antimony, arsenic and rare metal lanthanum, cerium; Allot the alloy cementing agent of 2Kg according to the prescription of above-mentioned plumbous antimony rare earth alloy cementing agent,
(2) baker: crucible temperature is set as 200 ℃, adds a small amount of charcoal and carry out baker, furnace drying time is 1h, keeps the crucible inner drying, without other impurity;
(3) preparation plumbum rare earth alloy intermediate: when furnace temperature reaches 200 ℃, add plumbous 160g, continue to be heated to 370 ℃, stopped heating insulation 12 minutes; Continue to be warming up to 920 ℃; Add 6g lanthanum and 2g cerium, drag for slag after continuing stirring and being incubated 20 minutes; Then cool to room temperature.
(4) preparation alloy cementing agent: dry boiler is heated to 200 ℃, then to the antimony and the arsenic that wherein add in remaining lead and the prescription, in dry boiler, adds wood charcoal powder simultaneously, then be heated to 600 ℃, remain that wood charcoal powder covers liquid level; Under this temperature, be incubated and stirred 5 minutes, form uniform plumbous antimony arsenic liquation; Add the plumbum rare earth alloy intermediate, all after the fusing, after insulation under this temperature and stirring 40 minutes, add 5% paraffin of plumbous antimony rare earth alloy total mass, then the rear slagging-off that stirs is incubated 15min and obtains the alloy cementing agent, then carries out insulator cementing.Stay a part of alloy sample calorimetric coefficient of expansion.
Particle diameter plumbous and antimony is 10～20mm, and the particle diameter of arsenic, lanthanum and cerium is 1～2mm; 80 ℃/h of all heat-up rate controls in the preparation process; Alr mode is to be pitch time 2min, and each churning time is 3min.
Embodiment 5: substantially the same manner as Example 1, difference is the proportioning raw materials of plumbous antimony rare earth alloy cementing agent: lead 90.0%, antimony 9.3%, arsenic 0.3%, lanthanum 0.2% and cerium 0.2%.
Embodiment 6: substantially the same manner as Example 1, difference is the proportioning raw materials of plumbous antimony rare earth alloy cementing agent: lead 91.2%, antimony 8.5%, arsenic 0.2%, lanthanum 0.1%.
In addition, the prescription of simultaneous test 1 is the plumbous antimony arsenic alloy cementing agent of referenced patent 200510041232.2, and simultaneous test 2 is plumbous antimony arsenical copper cementing agents of referenced patent 201210265774.8.
Employing is similar to the method test thermal expansivity of GB/T8411.2-2008 " pottery and vitreous insulating material part 2: test method ", and the contrast test data of each embodiment and existing cementing agent are as shown in the table:
Can see from upper table, mix a certain proportion of rare-earth elements of lanthanum and cerium (or only having lanthanum), reduce the thermal expansivity of alloy, make its connection porcelain piece and metal-ware of more closing, best proportioning is embodiment 1.
Above-described embodiment does not limit the present invention in any form, and all employings are equal to replaces or technical scheme that the mode of equivalent transformation obtains, all drops in protection scope of the present invention.
Claims (7)
1. a plumbous antimony rare earth alloy cementing agent is characterized in that, its prescription comprises that the weight percent of following component and each component is:
Plumbous 87.0 ~ 92.0%;
Antimony 7.0 ~ 12.0%;
Arsenic 0.1 ~ 0.5%;
Lanthanum 0.1 ~ 0.5%;
Cerium 0.0 ~ 0.2%.
2. the preparation method of a kind of plumbous antimony rare earth alloy cementing agent according to claim 1 is characterized in that, may further comprise the steps:
(1) gets the raw materials ready: prepare metallic lead, antimony, arsenic and rare metal lanthanum, cerium according to plumbous antimony rare earth alloy prescription claimed in claim 1;
(2) baker: crucible temperature is set as 200 ℃, adds a small amount of charcoal and carry out baker, furnace drying time is 0.8 ~ 1h, keeps the crucible inner drying, without other impurity;
(3) preparation plumbum rare earth alloy intermediate: when furnace temperature reaches 200 ℃, add lead, continue to be heated to 350 ~ 400 ℃, stopped heating insulation 10 ~ 15 minutes; Continue to be warming up to 920 ℃; Add rare earth lanthanum, cerium, drag for slag after continuing stirring and being incubated 20 minutes; Then cool to room temperature; Namely make the plumbum rare earth alloy intermediate;
(4) preparation alloy cementing agent: dry boiler is heated to 200 ℃, then to wherein adding remaining lead, antimony and arsenic, in dry boiler, adds wood charcoal powder simultaneously, then be heated to 550 ~ 600 ℃, remain that wood charcoal powder covers liquid level; Under this temperature, be incubated and stirred 2 ~ 5 minutes, form uniform plumbous antimony arsenic liquation; Add the plumbum rare earth alloy intermediate that makes in the step (3), all after the fusing, after insulation under this temperature and stirring 30 ~ 40 minutes, 1 ~ 5% the paraffin that adds plumbous antimony rare earth alloy total mass, rear slagging-off stirs, then be incubated 15 ~ 20min and obtain the alloy cementing agent, then carry out insulator cementing.
3. the preparation method of a kind of plumbous antimony rare earth alloy cementing agent according to claim 2 is characterized in that, the lead described in the step (1) and the particle diameter of antimony are 10 ~ 20mm, and the particle diameter of arsenic, lanthanum and cerium is 1 ~ 2mm.
4. the preparation method of a kind of plumbous antimony rare earth alloy cementing agent according to claim 2, it is characterized in that, in the process of step (3) preparation plumbum rare earth alloy intermediate, lead: the weight ratio of (lanthanum+cerium) is 50:1 ~ 20:1, and the per-cent that cerium accounts for lanthanum cerium quality is not more than 50%.
5. the preparation method of a kind of plumbous antimony rare earth alloy cementing agent according to claim 2 is characterized in that, 50 ~ 100 ℃/h of all heat-up rate controls in step (2), step (3) and the step (4).
6. the preparation method of a kind of plumbous antimony rare earth alloy cementing agent according to claim 2 is characterized in that, it is 2min that the stirring insulating process in step (3) and the step (4) requires the mixing chamber interval, and each churning time is 2 ~ 3min.
7. the application of alloy cementing agent according to claim 1 in insulator cementing.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63123594A (en) * | 1986-11-12 | 1988-05-27 | Toshiba Corp | Alloy for low temperature joining |
| CN1727504A (en) * | 2005-07-25 | 2006-02-01 | 叶胜平 | Lead antimony alloy of agglutiant in sue for insulator in transmission and transform circuit line, and preparation method |
| CN102787255A (en) * | 2012-07-30 | 2012-11-21 | 江苏南瓷绝缘子有限公司 | Alloy cement formula and preparation method and application thereof |
-
2013
- 2013-07-04 CN CN201310279919.4A patent/CN103374670B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63123594A (en) * | 1986-11-12 | 1988-05-27 | Toshiba Corp | Alloy for low temperature joining |
| CN1727504A (en) * | 2005-07-25 | 2006-02-01 | 叶胜平 | Lead antimony alloy of agglutiant in sue for insulator in transmission and transform circuit line, and preparation method |
| CN102787255A (en) * | 2012-07-30 | 2012-11-21 | 江苏南瓷绝缘子有限公司 | Alloy cement formula and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 杨兰生 等: "稀土对超低锑铅合金组织及性能的影响", 《天津大学学报》 * |
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