CN1278017A - Method and equipment for preparing yellow Dumet wire made of copper alloy - Google Patents
Method and equipment for preparing yellow Dumet wire made of copper alloy Download PDFInfo
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- CN1278017A CN1278017A CN 00112365 CN00112365A CN1278017A CN 1278017 A CN1278017 A CN 1278017A CN 00112365 CN00112365 CN 00112365 CN 00112365 A CN00112365 A CN 00112365A CN 1278017 A CN1278017 A CN 1278017A
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Abstract
The present invention relates to a preparation method of Domet wire and the improvement of its device. It changes controlles oxidation into controlled oxidation, to make the annelaing of Domet wire under reduction atomosphere, the hot Domet wire during or after annelaing is oxidized for a short time to produce cuprous oxide; after a thin layer of cuprous oxide is obtained, it is controlled that no further cuprous oxide is produced, and thereby an orange-coloured Domet wire with thin layer cuprous oxide is obtained.
Description
The present invention relates to electron tube in a kind of electric light source and the semicon industry, semiconducter device outlet line---the preparation method and the device of yellow Dumet wire made of copper alloy.
Last anneal oxidation in the Dumet wire manufacturing process adopts multiple boron high temperature natural oxidation in annealing process usually, makes the Dumet wire surface generate the good Red copper oxide protective layer of one deck chemical stability.The Red copper oxide protective layer that does not have the acquisition of control natural oxidation is general relative thicker, makes the Dumet wire appearance take on a red color or scarlet, and this Dumet wire with thicker Red copper oxide is called red Dumet wire traditionally, and the red more Red copper oxide layer that shows of Dumet wire color is thick more.Because for poor, thereby red Dumet wire connects at electricity and occur rosin joint, dry joint when connecing seal wire on the guiding machine easily far beyond copper for Red copper oxide electroconductibility and weldability, the coarse defective such as rough of solder joint seriously influences bulb quality.In addition because Red copper oxide has certain fragility, the blocked up Red copper oxide in Dumet wire surface twists in connecing a technology and is easy to be directed at Red copper oxide when vertical pulling is stretched and peels off (being commonly called as shedding), thereby destroyed the surface smoothness of Dumet wire, be directed at the Dumet wire downgrade, seriously influence the resistance to air loss of bulb, reduce bulb service life.Therefore thick Red copper oxide is directed at electricity and connects seal wire and pay no attention to and think of shedding two big defectives, is the deadly defect of raising Dumet wire quality.
For overcoming above-mentioned prior art deficiency; improve the electroconductibility on Dumet wire top layer; thereby improve electricity and connect the seal wire weldability; prevent the top layer powder that falls, Chinese patent 93105063 proposes a kind of formation at the thick metallic nickel of naked core silk electroplating surface 1-4 μ or materials such as silver, silver-bearing copper and has chemical stability and all good protective layer of electroconductibility.Yet this Dumet wire plating nickel on surface, silver or silver-bearing copper material, the one, the processing requirement height, production practice are difficult to control, and the final product rate is low; The 2nd, this technology has strengthened the manufacturing cost of Dumet wire, lacks actual application value.
The objective of the invention is to overcome the deficiency of above-mentioned prior art; provide a kind of may command Red copper oxide to generate; can obtain having Dumet wire manufacturing (anneal oxidation) technology of thin Red copper oxide (being orange) protective layer; make the Dumet wire that makes have good electroconductibility and weldability; the powder that do not fall is good with the glass head seal resistance to air loss.
Another object of the present invention is to provide a kind of adaptation above-mentioned technology purpose, manufacturing Dumet wire (anneal oxidation) device that may command Red copper oxide generates.
The present invention is for overcoming above-mentioned existing problems, the Red copper oxide that the Dumet wire surface is generated is thin as far as possible, basic design of the present invention is Dumet wire to be annealed make surface oxide layer reduction becoming copper under reducing atmosphere, then hot Dumet wire generates Red copper oxide by oxidation in short-term in annealing process or afterwards after answering boron, i.e. control does not allow it continue oxidation again and generates new Red copper oxide after Red copper oxide generates, and is bisque Dumet wire thereby obtain thin Red copper oxide.According to above-mentioned design, process reform annealing nothing of the present invention is controlled and has been oxidized to the control oxidation, by artificial controlled oxidation, obtains oxide thin layer cuprous back control and does not reoxidize, and overcoming does not have the blocked up disadvantage of bringing of the oxidation of control generation Red copper oxide.Specifically, the preparation method of yellow Dumet wire made of copper alloy of the present invention comprises throwing, anneal oxidation, it is characterized in that said anneal oxidation technology follows these steps to carry out: a, naked silk heat under reducing atmosphere; B, multiple boron; C, heating and controlled oxidation; D, cooling fast.
The said naked silk of the present invention heats under reducing atmosphere, its effect is that silk is heated under reducing atmosphere, hot silk not only can be removed the organic contamination that the surface is stained with, and reducing atmosphere makes Dumet wire be reduced to copper at the cupric oxide that the manufacturing processed mesexine produces, this generates attenuate Red copper oxide, and the quality that improves Dumet wire is favourable.Said reducing atmosphere is meant that Dumet wire silk surface in heat-processed is in the reducing atmosphere, and for example silk outside being reduced property gas such as hydrogen, CO (carbon monoxide converter) gas are wrapped up.The said multiple boron of the present invention is undertaken by common technology, has no special requirements.Said heating and controlled oxidation are meant the oxidizing reaction of multiple boron filament artificial control Dumet wire and oxygen in the subsequent anneal process, make the cuprous generation of a surface oxidation not make it blocked up to be orange for well.Heating and controlled oxidation can be that heating anneal carries out in well-oxygenated environment (contact with air or lead to oxygen) earlier, then in oxygen barrier environment (for example the Dumet wire outside is with the protection of nitrogen or other oxygenless gas), carry out, do not make to contact oxygen again in its annealing process after oxidation and oxidation takes place generate new Red copper oxide; Can be first heating anneal also, control oxidation in short-term after coming out of the stove and make the top layer generate thin Red copper oxide.Oxidation can be to carry out in air, also can be to carry out in logical oxygen environment.The heating controlled oxidation its objective is in the heating anneal process control and oxygen duration of contact, thereby reaches the cuprous generation thickness of controlled oxidation (amount).Said quick cooling is to make to generate the cuprous Dumet wire of oxide thin layer and cool off rapidly, does not make it reoxidize in follow-up receipts silk process that to produce excessive oxidation cuprous, reaches the cuprous growing amount of controlled oxidation.For guaranteeing not reoxidize in the follow-up receipts silk process, cooling preferably continues to carry out in the oxygen barrier environment, simultaneously for Dumet wire can be cooled to rapidly below the oxidizing temperature, the mode of a kind of less expensive of cooling is for adopting the water proof cooling fast, be about to the Dumet wire water proof and pass water layer, make it to be cooled off fast, both economical effectiveness might as well.
Be to guarantee the quality of Dumet wire, annealing temperature can be taked the annealing process that progressively improves, so both can avoid that the silk surface generates too much Red copper oxide in annealing process, meets the unit elongation of annealing and obtaining suiting again.Reduced anneal silk temperature of the present invention is comparatively suitable with 680-750 ℃, and subsequent anneal silk temperature is comparatively suitable with 800-980 ℃.Said temperature is not the extreme value scope, and Si Wen is relevant with wire travelling speed, annealing furnace length etc.
According to anneal oxidation technology of the present invention, the present invention makes the device of yellow Dumet wire made of copper alloy, comprise the annealing furnace of built-in seal wire boiler tube and soak the boron groove, said annealing furnace is by preceding preheating oven and retreat stove and form, the said boron groove that soaks is between two stoves, it is characterized in that said preheating oven wire leading pipe front end has a gas introduction port, the rear end has gas to derive " chimney ", said annealing furnace wire leading pipe middle part has gas to derive " chimney ", end does not have gas introduction port, there is the water-chilling plant of band wire leading pipe said annealing furnace rear end, and the wire leading pipe of said water-chilling plant links to each other with the annealing furnace wire leading pipe.
According to anneal oxidation technology of the present invention, the device that the present invention makes yellow Dumet wire made of copper alloy can also be, comprise the annealing furnace of built-in seal wire boiler tube and soak the boron groove, said annealing furnace is by preceding preheating oven and retreat stove and form, the said boron groove that soaks is characterized in that said preheating oven wire leading pipe front end has a gas introduction port between two stoves, the rear end has gas to derive " chimney ", be interval with the water-chilling plant of band wire leading pipe behind the said annealing furnace, there is gas introduction port at water-chilling plant wire leading pipe middle part.Wherein annealing furnace and water-chilling plant are better at interval with 1-5cm, are more preferred from 1-2cm, and at this moment the Red copper oxide of Sheng Chenging is comparatively suitable.Annealing furnace and water-chilling plant interbody spacer can be to be interrupted, even Dumet wire exposed to air natural oxidation; Can also be to link to each other, oxidation is carried out in logical oxygen environment at the oxygen-supplying tube of interval section with band gas introduction port and derivation " chimney ".
Below in conjunction with the description of two indefiniteness embodiment, further specify the inventive method and device.
Fig. 1 is that embodiment 1 makes yellow Dumet wire made of copper alloy anneal oxidation apparatus structure synoptic diagram.
Fig. 2 is that embodiment 2 makes yellow Dumet wire made of copper alloy anneal oxidation apparatus structure synoptic diagram.
Embodiment 1: referring to Fig. 1, the anneal oxidation device is made up of the preheating oven 4 and the annealing furnace 7 of built-in porcelain or pyroceram seal wire boiler tube 2, be provided with between preheating oven and annealing furnace and soak boron groove 6, in concentration is arranged is the 16-18% borate, there is the water cooling case 11 of band wire leading pipe 2 the annealing furnace rear end, for improving speed of cooling, water-cooled case wire leading pipe is done by metal such as copper, and water-cooled case wire leading pipe links to each other with the annealing furnace wire leading pipe.Preheating oven wire leading pipe front end has hydrogen introducing port 3, the rear end has hydrogen to derive " chimney " 5, annealing furnace wire leading pipe middle part has gas to derive " chimney " 8, and end does not have gas introduction port 9, has pneumatic outlet 10 about annealing furnace wire leading pipe " chimney " portion and forms the gas passage with " chimney ".About preheating furnace superintendent 75cm, about annealing furnace superintendent 150cm.
It during anneal oxidation is the naked silk 1 of copper with the top layer, send into and make the silk temperature be reduction in 680-750 ℃ the preheating oven 4, hydrogen is entered by gas introduction port 3 and is full of wire leading pipe by " chimney " 5 discharges, full hydrogen makes Dumet wire be in heating in the reducing gas parcel in the wire leading pipe, Dumet wire is removed by its surperficial zone of oxidation of preheating oven and the organic dirt that is stained with, obtains the surface and is the Dumet wire of non-oxidation copper.By soaking the multiple boron of boron groove, heated filament makes multiple last layer in silk surface and thin borax solution by the boron liquid bath after the reductive Dumet wire is come out of the stove.The Dumet wire that breaks away from boron liquid enters annealing furnace 7 oxidizing annealings, the nitrogen that middle part " chimney " and rear portion gas introduction port 9 feeds, and making annealing furnace anterior is oxidation zone, the rear portion is the oxygen barrier district.The silk temperature of control " chimney " 8 front ends be 800-900 ℃, and this moment, Dumet wire at high temperature the oxidizing reaction generation took place than the Red copper oxide (but also oxygen oxidation) that approaches with contact by the oxygen in the seal wire air in tube; The silk temperature of control " chimney " 8 rear ends is about 900-980 ℃; when the Dumet wire that the existing Red copper oxide in surface this moment generates continues annealing in this district; because nitrogen protection causes the oxygen barrier environment, Dumet wire at high temperature can not continue oxidation again by this district yet and generate new Red copper oxide.The boron liquid on silk surface forms one deck glass integument because of high temp glassization on the silk surface in annealing process simultaneously.Dumet wire goes out the cooling water tank that enters mobile cold water behind the annealing furnace, and to be quickly cooled to the following as silk temperature of oxidizing temperature be about 60 ℃, silk is entered by the cooling water tank wire leading pipe by introducing port 9 and is not held the nitrogen of discharge to be wrapped up in process of cooling, so also can not continue oxidation in the process of cooling.The silk temperature is low early and high after in the oxidizing annealing, to the cuprous formation speed of controlled oxidation, guarantees to generate thin Red copper oxide and guarantee that suitable unit elongation is favourable.
Embodiment 2: referring to Fig. 2 as described above, wherein annealing furnace 7 is discontinuous with water cooling case 11, and the 1-2cm gap is arranged therebetween, and there is gas introduction port 12 at water cooling case wire leading pipe middle part.
As described above, multiple boron filament enters annealing in the annealing furnace 7, and the annealing furnace temperature is low early and high after, make the silk temperature 800 to 980 ℃ of scopes, because the annealing furnace temperature is higher, wire leading pipe does not have " chimney " again and forms gas stream, thereby because no capacity air, Dumet wire is less in annealing furnace to have Red copper oxide to generate.The high temperature silk of coming out of the stove contacts with air oxidation takes place, and makes the silk surface generate one deck Red copper oxide, and it is very short that the Yin Gaowen heated filament exposes in the air time to the open air, thereby the Red copper oxide that generates is also less relatively.Generation has the hot Dumet wire of Red copper oxide to enter cooling water tank immediately to cool off fast, the nitrogen that the gas introduction port 12 at cooling water tank wire leading pipe middle part feeds is derived by the wire leading pipe two ends, Dumet wire is in the oxygen barrier environment in process of cooling again like this, do not have again new Red copper oxide to generate yet, thereby guaranteed the thin Red copper oxide in silk surface.
Annealing device wire leading pipe one of the present invention effect is full gas, and the silk place is given in the specific gas parcel, and it is full and flow additional that the effect of " chimney " then helps gas it on.
Temperature parameter that the present invention provides and furnace superintendent are not one to be decided to be the extreme value scope, link mutually between silk temperature, furnace superintendent, the wire travelling speed, can change.
The Dumet wire that the inventive method makes is compared with the Dumet wire that prior art makes has following advantage and good effect: this Method can generate thickness to Dumet wire top layer cuprous oxide and control, and it is thinner to be easy to obtain the cuprous layer of surface oxidation, is orange The Dumet wire of look, thus overcome the end of keeping away that former thicker cuprous oxide brings, powder falling not, top layer good conductivity, electric fusion welding The property raising, solder joint is smooth firmly, with this make electron tube, electric guide wire air-tightness is good, can not leak air, greatly carry The high qualification rate of seal. Apparatus of the present invention are simple in structure, and production effect is good.
Claims (10)
1, a kind of preparation method of yellow Dumet wire made of copper alloy comprises throwing, anneal oxidation, it is characterized in that said anneal oxidation technology follows these steps to carry out:
A, naked silk heat under reducing atmosphere;
B, multiple boron;
C, heating and controlled oxidation;
D, cooling fast.
2,, it is characterized in that said reducing atmosphere is logical hydrogen shield according to the preparation method of the described yellow Dumet wire made of copper alloy of claim 1.
3, according to the preparation method of the described yellow Dumet wire made of copper alloy of claim 1, it is characterized in that said heating and controlled oxidation are the heat-processed initial oxidation, then under the oxygen barrier environment, continue heating.
4,, it is characterized in that said annealing silk temperature improves gradually 680-980 ℃ of scope according to the preparation method of the described yellow Dumet wire made of copper alloy of claim 1.
5,, it is characterized in that the said water proof cooling that is cooled to fast according to the preparation method of the described yellow Dumet wire made of copper alloy of claim 1.
6,, it is characterized in that said water proof process of cooling carries out in the oxygen barrier environment according to the preparation method of the described yellow Dumet wire made of copper alloy of claim 5.
7,, it is characterized in that said oxygen barrier environment is logical nitrogen protection according to the preparation method of claim 3 or 6 described yellow Dumet wire made of copper alloy.
8, a kind of anneal oxidation device of making yellow Dumet wire made of copper alloy, comprise the annealing furnace of built-in seal wire boiler tube and soak the boron groove, said annealing furnace is by preceding preheating oven and retreat stove and form, the said boron groove that soaks is between two stoves, it is characterized in that said preheating oven wire leading pipe front end has a gas introduction port, the rear end has gas to derive " chimney ", there is gas derivation " chimney " at said annealing furnace wire leading pipe middle part, end does not have gas introduction port, there is the water-chilling plant of band wire leading pipe said annealing furnace rear end, and the wire leading pipe of said water-chilling plant links to each other with the annealing furnace wire leading pipe.
9, a kind of anneal oxidation device of making yellow Dumet wire made of copper alloy, comprise the annealing furnace of built-in seal wire boiler tube and soak the boron groove, said annealing furnace is by preceding preheating oven and retreat stove and form, the said boron groove that soaks is between two stoves, it is characterized in that said preheating oven wire leading pipe front end has a gas introduction port, the rear end has gas to derive " chimney ", is interval with the water-chilling plant of band wire leading pipe behind the said annealing furnace, and there is gas introduction port at water-chilling plant wire leading pipe middle part.
10,, it is characterized in that said annealing furnace and water-chilling plant are spaced apart 1-5cm according to the device of the yellow Dumet of the described manufacturing of claim 9.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00112365 CN1278017A (en) | 2000-06-30 | 2000-06-30 | Method and equipment for preparing yellow Dumet wire made of copper alloy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00112365 CN1278017A (en) | 2000-06-30 | 2000-06-30 | Method and equipment for preparing yellow Dumet wire made of copper alloy |
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| CN1278017A true CN1278017A (en) | 2000-12-27 |
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| CN 00112365 Pending CN1278017A (en) | 2000-06-30 | 2000-06-30 | Method and equipment for preparing yellow Dumet wire made of copper alloy |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103474400A (en) * | 2013-09-14 | 2013-12-25 | 许晗 | Boron-free oxidation dumet wire and manufacturing processes thereof |
| CN108239738A (en) * | 2016-12-26 | 2018-07-03 | 无锡佳力欣精密机械有限公司 | For the technique to the jaundice processing of copper-based axial bearing surface |
| CN108326473A (en) * | 2017-07-31 | 2018-07-27 | 江西金世纪特种焊接材料有限公司 | A kind of process of surface treatment of phosphor-copper class brazing material |
| CN111013970A (en) * | 2018-10-10 | 2020-04-17 | 江苏昆仑光源材料有限公司 | Oxidation, sintering and film coating integrated device for producing high-purity Dumet wire coating layer |
-
2000
- 2000-06-30 CN CN 00112365 patent/CN1278017A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103474400A (en) * | 2013-09-14 | 2013-12-25 | 许晗 | Boron-free oxidation dumet wire and manufacturing processes thereof |
| WO2015035682A1 (en) * | 2013-09-14 | 2015-03-19 | Jin Jiashan | Boron-free oxide dumet wire and manufacturing process therefor |
| CN108239738A (en) * | 2016-12-26 | 2018-07-03 | 无锡佳力欣精密机械有限公司 | For the technique to the jaundice processing of copper-based axial bearing surface |
| CN108326473A (en) * | 2017-07-31 | 2018-07-27 | 江西金世纪特种焊接材料有限公司 | A kind of process of surface treatment of phosphor-copper class brazing material |
| CN111013970A (en) * | 2018-10-10 | 2020-04-17 | 江苏昆仑光源材料有限公司 | Oxidation, sintering and film coating integrated device for producing high-purity Dumet wire coating layer |
| CN111013970B (en) * | 2018-10-10 | 2024-05-17 | 江苏昆仑光源材料有限公司 | Oxidation, sintering and film coating integrated device for producing high-purity Dumet wire coating layer |
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