CN100541944C - A kind of manufacture method of electric heater socket connector plug - Google Patents
A kind of manufacture method of electric heater socket connector plug Download PDFInfo
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- CN100541944C CN100541944C CNB2006101195002A CN200610119500A CN100541944C CN 100541944 C CN100541944 C CN 100541944C CN B2006101195002 A CNB2006101195002 A CN B2006101195002A CN 200610119500 A CN200610119500 A CN 200610119500A CN 100541944 C CN100541944 C CN 100541944C
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Abstract
The present invention relates to a kind of manufacture method of electric heater socket connector plug, this method comprises following processing step: the preparation of (1) metallization slurry, and (2) slurry coating, (3) metallization sintering, (4) glazing and gloss firing, electroplate (5), (6) soldering.Compare with conventional art, the present invention adopts ceramic metallization and process for sealing, by adjusting the formula of size of metal molybdenum, manganese, improve sintering method and method for sealing, and utilize the corrosion resistance and the good characteristic of electrical insulating property of ceramic material, make this connector have anticorrosion, heatproof, anti-irradiation, the characteristics that air-tightness and electrical insulation capability are good in the useful life that can improve electric heater, reduce product cost.
Description
Technical field
The present invention relates to a kind of ceramic metallization process for sealing, relate in particular to the ceramic metallization method for sealing of electric heater socket connector.
Background technology
That pottery has is high temperature resistant, radiation hardness, air-tightness are good, electrical insulation capability is good, by special solder technology pottery and metal are coupled together, China begins to adopt this technology at electron tube from the fifties, development is very fast, has grasped the welding method of sintering metal powder method and active metallization method soon.The ceramic-metal sealing-in solder technology of China has been applied in many industries now, has also entered the stage of designing and developing new material, new method voluntarily from experimental study, application.Along with the development of electronics industry and nuclear energy, many products all adopt the ceramic-metal sealing technology to make production.At present, the sintering metal powder method is one of mature technique, at first ceramic surface is adopted the metallization of sintering metal powder, and then and metal carry out soldering, pottery and metal are coupled together.Wherein concrete method has Mo-Mn method, active Mo-Mn method, W-Fe method or the like.
Because the kind of pottery has a lot, and is also different according to metallization component and method that different materials is used, must make metal dust and ceramic base material well sintering be in the same place, have certain intensity, could satisfy specification requirement.At present, the molybdenum manganese metal is a kind of mature methods, but complex process, and cost of manufacture is higher, and the metal layer bond strength is low.
Summary of the invention
Purpose of the present invention is exactly that a kind of technology that provides for the defective that overcomes above-mentioned conventional art existence is simple, and cost is low, the manufacture method of the electric heater socket connector plug that the metal layer bond strength is high.
Purpose of the present invention can be achieved through the following technical solutions: a kind of manufacture method of electric heater socket connector plug, it is characterized in that this method adopts the ceramic metallization process for sealing, and this method comprises following processing step:
(1) preparation of metallization slurry
Dispose raw material by following component and content (percentage by weight):
Molybdenum powder: 50～65%;
Manganese powder: 15～25%;
Additive: 15～20%;
Solvent: 2～10%;
Four kinds of components are put into the nominal ball grinder of ball milling, and ball milling is 2～5 hours in ball mill, obtains molybdenum manganese metal paste;
(2) slurry coating
The earthenware that cleans, oven dry is good is placed on the whirligig, according to drawing require earthenware require position paint metals slurry, coat the back airing, the metalized coated thickness in dry back is 50～80 μ m;
(3) metallization sintering
The earthenware that starching is good is placed on the molybdenum boat, places the high temperature hydrogen furnace sintering, and under the wet hydrogen protective atmosphere, sintering temperature is controlled at 1400～1550 ℃, is incubated 40～60 minutes, and earthenware is taken out in cooling then;
(4) glazing and gloss firing
Do not have metallized surface to carry out glazing on earthenware, oven dry places high temperature hydrogen furnace to carry out gloss firing, and under hydrogen shield atmosphere, the gloss firing temperature is controlled at 1200～1300 ℃, is incubated 10～20 minutes;
(5) electroplate
Step (4) gained metallized ceramic pipe is carried out nickel plating;
(6) soldering
With earthenware and can cut down, metal patches loop bar, stainless steel connector base installing and locating by drawing; silver solder is fixed on the welding position, in soldering oven, carries out soldering, in hydrogen shield atmosphere; be warming up to 950～1100 ℃, be incubated 10～15 minutes.
The granularity of described molybdenum powder, manganese powder is 200～360 orders.
Described earthenware adopts aluminium oxide ceramics.
Described solvent is with guncotton solution and ethyl acetate, guncotton is put into ethyl acetate heat, and it is dissolved fully becomes solvent, and its component weight proportion is: ethyl acetate: 90～95%; Guncotton: 5～10%.
Described additive comprises alumina powder, calcium oxide powder, silica powder.
The nickel plating of described metallized ceramic pipe, the electroplate liquid component is as follows by weight ratio:
Ingredients weight parts
100 parts of nickelous sulfates;
25～35 parts in sodium sulphate;
20～30 parts in magnesium sulfate;
10～20 parts of boric acid;
3～6 parts in sodium chloride.
Described electroplate liquid is prepared with deionized water, and uses the washed with de-ionized water plating piece.
The present invention improves sintering method by adjusting the prescription of molybdenum manganese metal slurry, and a soldering is finished, and has reduced the cost of manufacture of product, and the rupture strength of ceramic weldment is at 8000～10000N/cm
2Compare with conventional art, the present invention has the following advantages: the bond strength height of its ceramic metallization sintering, the device of in this way making has anticorrosion, heatproof, anti-irradiation, air-tightness and electrical insulation capability are good, and it can have medium-term and long-term the use and the maintenance good electrical properties of environment of radiation at 150 ℃ of temperature, pressure 0.6Mpa.The connector that adopts the ceramic metallization method for sealing to make has changed former nuclear power plant voltage stabilizer and can't change separately after aging with the cable of electric heater, situation about must change together with electric heater.Prolong the useful life of electric heater, reduced operation, the maintenance cost of the nuclear power station of nuclear power station, shortened maintenance time, solved the problem of changing cable, had better economic.
Description of drawings
Fig. 1 is the structural representation of electric heater socket connector metallization sealing-in of the present invention.
Embodiment
The present invention adopts the ceramic metallization process for sealing to make electric heater socket connector, is described further by embodiment below in conjunction with accompanying drawing, comprises among the figure that first can cut down 1, stainless steel connector base 2, and metallized ceramic pipe 3, the second can cut down 4, and metal patches loop bar 5.
Embodiment 1
As shown in Figure 1, a kind of employing ceramic metallization method for sealing is made electric heater socket connector, can be used for the tubular electric heating of particular surroundings such as chemical industry.Adopt ceramic metallization and method for sealing technology, by adjusting the formula of size of metal molybdenum, manganese, improve sintering method and method for sealing, and utilize the corrosion resistance and the good characteristic of electrical insulating property of ceramic material, make this connector have anticorrosion, heatproof, anti-irradiation, the characteristics that air-tightness and electrical insulation capability are good, can improve the useful life of electric heater, reduce product cost.The concrete grammar step is as follows:
(1) preparation of metallization slurry
Get 300 purpose molybdenum powders 500 gram, 300 purpose manganese powders, 500 grams, 300 purpose additives, 500 grams, ball milling after 12 hours in ball mill is stand-by respectively.The 200ml ethyl acetate is poured in the port grinding bottle of 500ml, and added 50 gram guncottons stirrings, guncotton all dissolves after 24 hours, and is standby.From the material that grinds, take by weighing 200 gram molybdenum powders, 100 gram manganese powders, 120 gram additives and 30 gram solvents, ball milling mixed 3 hours in ball grinder.After this, the slurry that will metallize is poured in the glassware standby.
(2) slurry coating
The earthenware that cleans, oven dry is good is placed on the whirligig, requires to adopt manual brushing, coat the back airing at the position that requires of earthenware according to drawing.Metallization slurry coating layer thickness is 0.08mm.
(3) metallization sintering
The earthenware that coats the metallization slurry is placed on the molybdenum boat, places vertical hydrogen furnace, logical nitrogen; logical again hydrogen is lighted to the stove gas outlet, and the wet hydrogen Buchholz protection is used in hydrogen furnace energising intensification during furnace temperature to 1200 ℃; to 1450 ℃ of insulations 60 minutes, earthenware was taken out in cooling then.The situation of metallization sintering is seen in check, all will detect if any bubble, be full of cracks, removes as defective item.
(4) electroplate
Put into the 4000ml deionized water with chemical pure nickelous sulfate 600 gram, take by weighing 250 gram sodium sulphate and 100 gram magnesium sulfate, boric acid 60 grams, sodium chloride 20 grams are put into solution, are stirred to dissolving fully.
With the effective sand papering of metallized ceramic, the pH value is 5, and the current density of plating is 1.0A/dm2, electroplating time 40min, and thickness of coating is 8 μ m.
(5) soldering
With earthenware and can cut down, metal patches loop bar, stainless steel connector base installing and locating by drawing, and silver solder is fixed on the welding position, carries out soldering in soldering oven, is warming up to 950 ℃, be incubated 10 minutes, cool off.Make socket connector plug, and carry out leakage test and electric performance test, to guarantee the sealing and the electrical insulating property of plug.
Embodiment 2
(1) preparation of metallization slurry
Get 300 purpose molybdenum powders 500 gram, 300 purpose manganese powders, 500 grams, 300 purpose additives, 500 grams, ball milling after 12 hours in ball mill is stand-by respectively.The 285g ethyl acetate is poured in the port grinding bottle of 500ml, and added 15 gram guncottons stirrings, guncotton all dissolves after 24 hours, and is standby.From the material that grinds, take by weighing 250 gram molybdenum powders, 125 gram manganese powders, 100 gram additives and 25 gram solvents, ball milling mixed 5 hours in ball grinder.After this, the slurry that will metallize is poured in the glassware standby.
(2) slurry coating
The earthenware that cleans, oven dry is good is placed on the whirligig, requires to adopt manual brushing, coat the back airing at the position that requires of earthenware according to drawing.Metallization slurry coating layer thickness is 0.05mm.
(3) metallization sintering
The earthenware that coats the metallization slurry is placed on the molybdenum boat, places vertical hydrogen furnace, logical nitrogen; logical again hydrogen is lighted to the stove gas outlet, and the wet hydrogen Buchholz protection is used in hydrogen furnace energising intensification during furnace temperature to 1200 ℃; to 1400 ℃ of insulations 60 minutes, earthenware was taken out in cooling then.The situation of metallization sintering is seen in check, all will detect if any bubble, be full of cracks, removes as defective item.
(4) glazing gloss firing
To there not being metallized surface to carry out glazing on the earthenware, oven dry places high temperature hydrogen furnace to carry out gloss firing, and under hydrogen shield atmosphere, the gloss firing temperature is controlled at 1300 ℃, is incubated 20 minutes.
(5) electroplate
Put into the 4000ml deionized water with chemical pure nickelous sulfate 1000 gram, take by weighing 250 gram sodium sulphate and 200 gram magnesium sulfate, boric acid 100 grams, sodium chloride 30 grams are put into solution, are stirred to dissolving fully.
With the effective sand papering of metallized ceramic, the pH value is 5, and the current density of plating is 1.0A/dm2, electroplating time 40min, and thickness of coating is 8 μ m.
(6) soldering
With earthenware and can cut down, metal patches loop bar, stainless steel connector base installing and locating by drawing, and silver solder is fixed on the welding position, carries out soldering in soldering oven, is warming up to 980 ℃, be incubated 15 minutes, cool off.Make socket connector plug, and carry out leakage test and electric performance test, to guarantee the sealing and the electrical insulating property of plug.
Embodiment 3
(1) preparation of metallization slurry:
Get 300 purpose molybdenum powders 500 gram, 300 purpose manganese powders, 500 grams, 300 purpose additives, 500 grams, ball milling after 12 hours in ball mill is stand-by respectively.The 270g ethyl acetate is poured in the port grinding bottle of 500ml, and added 30 gram guncottons stirrings, guncotton all dissolves after 24 hours, and is standby.From the material that grinds, take by weighing 325 gram molybdenum powders, 75 gram manganese powders, 75 gram additives and 25 gram solvents, ball milling mixed 2 hours in ball grinder.After this, the slurry that will metallize is poured in the glassware standby.
(2) slurry coating
The earthenware that cleans, oven dry is good is placed on the whirligig, requires to adopt manual brushing, coat the back airing at the position that requires of earthenware according to drawing.Metallization slurry coating layer thickness is 0.05mm.
(3) metallization sintering
The earthenware that coats the metallization slurry is placed on the molybdenum boat, places vertical hydrogen furnace, logical nitrogen; logical again hydrogen is lighted to the stove gas outlet, and the wet hydrogen Buchholz protection is used in hydrogen furnace energising intensification during furnace temperature to 1300 ℃; to 1550 ℃ of insulations 40 minutes, earthenware was taken out in cooling then.The situation of metallization sintering is seen in check, all will detect if any bubble, be full of cracks, removes as defective item.
(4) glazing gloss firing
To there not being metallized surface to carry out glazing on the earthenware, oven dry places high temperature hydrogen furnace to carry out gloss firing, and under hydrogen shield atmosphere, the gloss firing temperature is controlled at 1200 ℃, is incubated 10 minutes.
(5) electroplate
Put into the 4000ml deionized water with chemical pure nickelous sulfate 1000 gram, take by weighing 250 gram sodium sulphate and 200 gram magnesium sulfate, boric acid 100 grams, sodium chloride 30 grams are put into solution, are stirred to dissolving fully.
With the effective sand papering of metallized ceramic, the pH value is 5, and the current density of plating is 1.0A/dm2, electroplating time 40min, and thickness of coating is 8 μ m.
(6) soldering
With earthenware and can cut down, metal patches loop bar, stainless steel connector base installing and locating by drawing, and silver solder is fixed on the welding position, carries out soldering in soldering oven, is warming up to 980 ℃, be incubated 10 minutes, cool off.Make socket connector plug, and carry out leakage test and electric performance test, to guarantee the sealing and the electrical insulating property of plug.
Claims (7)
1. the manufacture method of an electric heater socket connector plug is characterized in that, this method adopts the ceramic metallization process for sealing, and this method comprises following processing step:
(1) preparation of metallization slurry
Dispose raw material by following component and content (percentage by weight):
Molybdenum powder: 50～65%;
Manganese powder: 15～25%;
Additive: 15～20%;
Solvent: 2～10%;
Four kinds of components are put into the nominal ball grinder of ball milling, and ball milling is 2～5 hours in ball mill, obtains molybdenum manganese metal paste;
(2) slurry coating
The earthenware that cleans, oven dry is good is placed on the whirligig, according to drawing require earthenware require position paint metals slurry, coat the back airing, the metalized coated thickness in dry back is 50～80 μ m;
(3) metallization sintering
The earthenware that starching is good is placed on the molybdenum boat, places the high temperature hydrogen furnace sintering, and under the wet hydrogen protective atmosphere, sintering temperature is controlled at 1400～1550 ℃, is incubated 40～60 minutes, and earthenware is taken out in cooling then;
(4) glazing and gloss firing
Do not have metallized surface to carry out glazing on earthenware, oven dry places high temperature hydrogen furnace to carry out gloss firing, and under hydrogen shield atmosphere, the gloss firing temperature is controlled at 1200～1300 ℃, is incubated 10～20 minutes;
(5) electroplate
Step (4) gained metallized ceramic pipe is carried out nickel plating;
(6) soldering
With earthenware and can cut down, metal patches loop bar, stainless steel connector base installing and locating by drawing; silver solder is fixed on the welding position, in soldering oven, carries out soldering, in hydrogen shield atmosphere; be warming up to 950～1100 ℃, be incubated 10～15 minutes.
2, the manufacture method of a kind of electric heater socket connector plug according to claim 1 is characterized in that, the granularity of described molybdenum powder, manganese powder is 200～360 orders.
3, the manufacture method of a kind of electric heater socket connector plug according to claim 1 is characterized in that, described earthenware adopts aluminium oxide ceramics.
4, the manufacture method of a kind of electric heater socket connector plug according to claim 1, it is characterized in that, described solvent is with guncotton solution and ethyl acetate, guncotton is put into ethyl acetate to be heated, it is dissolved fully becomes solvent, and its component weight proportion is: ethyl acetate: 90～95%; Guncotton: 5～10%.
5, the manufacture method of a kind of electric heater socket connector plug according to claim 1 is characterized in that, described additive comprises alumina powder, calcium oxide powder, silica powder.
6, the manufacture method of a kind of electric heater socket connector plug according to claim 1 is characterized in that, the nickel plating of described metallized ceramic pipe, and the electroplate liquid component is as follows by weight ratio:
Ingredients weight parts
100 parts of nickelous sulfates;
25～35 parts in sodium sulphate;
20～30 parts in magnesium sulfate;
10～20 parts of boric acid;
3～6 parts in sodium chloride.
7, the manufacture method of a kind of electric heater socket connector plug according to claim 6 is characterized in that, described electroplate liquid is prepared with deionized water, and uses the washed with de-ionized water plating piece.
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| CNB2006101195002A CN100541944C (en) | 2006-12-12 | 2006-12-12 | A kind of manufacture method of electric heater socket connector plug |
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| CNB2006101195002A CN100541944C (en) | 2006-12-12 | 2006-12-12 | A kind of manufacture method of electric heater socket connector plug |
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| CN100541944C true CN100541944C (en) | 2009-09-16 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102290305B (en) * | 2011-07-22 | 2013-11-27 | 安徽华东光电技术研究所 | Method for metalizing inner circle of long ceramic cylinder |
| CN102629504B (en) * | 2012-04-13 | 2013-10-30 | 中核能源科技有限公司 | Ceramic and metal sealed safety-level K1 class cable used in nuclear reactor |
| EP2851151B1 (en) * | 2013-09-20 | 2017-08-23 | Ansaldo Energia IP UK Limited | Method of fixing through brazing a heat resistant component on a surface of a heat exposed component |
| CN108314459A (en) * | 2017-01-16 | 2018-07-24 | 贵州天义电器有限责任公司 | Ceramics and binding post soldering connection process in a kind of sealing high voltage connector |
| CN109055891A (en) * | 2018-08-15 | 2018-12-21 | 娄底市安地亚斯电子陶瓷有限公司 | A kind of preparation method of power battery ceramic connector metalization layer |
| CN110061384A (en) * | 2019-04-24 | 2019-07-26 | 中广核研究院有限公司 | A kind of hermetically-sealed electrical connector |
| CN111192797A (en) * | 2020-01-22 | 2020-05-22 | 西北核技术研究院 | High-voltage large-current fuse sealing packaging method |
| CN113427097B (en) * | 2021-08-25 | 2021-12-14 | 西安远航真空钎焊技术有限公司 | Preparation method of wind tunnel heater containing special-shaped air pipe |
| CN114043029A (en) * | 2021-11-05 | 2022-02-15 | 天津航空机电有限公司 | Brazing method for welding molybdenum alloy and kovar alloy by using copper-platinum solder |
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- 2006-12-12 CN CNB2006101195002A patent/CN100541944C/en active Active
Non-Patent Citations (2)
| Title |
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| 95瓷金属化及上釉新工艺的研究. 周群等.中国核科技报告，第2007年02期. 2007 |
| 95瓷金属化及上釉新工艺的研究. 周群等.中国核科技报告，第2007年02期. 2007 * |
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Owner name: NUCLEAR INDUSTRY NO 8 INSTITUTE Effective date: 20140127 Owner name: STATE GRID SHANGHAI ELECTRIC POWER COMPANY Free format text: FORMER OWNER: NUCLEAR INDUSTRY NO 8 INSTITUTE Effective date: 20140127 |
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Effective date of registration: 20140127 Address after: 200002 Nanjing East Road, Shanghai, No. 181, No. Patentee after: State Grid Shanghai Municipal Electric Power Company Patentee after: Nuclear Industry No 8 Institute Address before: 201800, 1719 Jia Luo Road, Shanghai, Jiading District Patentee before: Nuclear Industry No 8 Institute |