CN1094810C - Active solder and its preparation - Google Patents

Active solder and its preparation Download PDF

Info

Publication number
CN1094810C
CN1094810C CN99124681A CN99124681A CN1094810C CN 1094810 C CN1094810 C CN 1094810C CN 99124681 A CN99124681 A CN 99124681A CN 99124681 A CN99124681 A CN 99124681A CN 1094810 C CN1094810 C CN 1094810C
Authority
CN
China
Prior art keywords
rolling
active solder
purity
sintering
blank
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN99124681A
Other languages
Chinese (zh)
Other versions
CN1258580A (en
Inventor
李元元
严志军
代明江
刘正义
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
South China University of Technology SCUT
Original Assignee
South China University of Technology SCUT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by South China University of Technology SCUT filed Critical South China University of Technology SCUT
Priority to CN99124681A priority Critical patent/CN1094810C/en
Publication of CN1258580A publication Critical patent/CN1258580A/en
Application granted granted Critical
Publication of CN1094810C publication Critical patent/CN1094810C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Ceramic Products (AREA)

Abstract

The present invention relates to Ag-Cu-Ti active solder and a metallurgic preparation method for solder powder. The alloy powder of the Ag-Cu-Ti active solder comprises the following components by the weight percentage range: 49 to 69 % of Ag, 30 to 50 % of Cu and 1 to 8 % of Ti; the welding rod is prepared by that the components are mixed, pressed, sintered in vacuum, annealed, rolled in a hot way and rolled in a cold way. The melting point of the Ag-Cu-Ti active solder offered by the present invention is from 780 to 830 DEG C, and the purity is larger than 99%. The present invention has the advantages of simple technology, economical use and wide application range; particularly, the present invention solves the problems which are difficult to overcome in the prior art. The present invention can be successfully used for welding adamas and metal, and welding ZrO2 ceramic and alloy steel; the welding quality is favorable, and the welding technology is simplified.

Description

A kind of preparation method of active solder
Technical field
The present invention relates to a kind of cored solder, specifically be meant a kind of preparation method who is used for the cored solder of diamond, pottery and metal (cutter) welding.
Background technology
In the welding procedure of existing diamond tool, the soldering of polycrystalline diamond instrument because the polycrystalline diamond sheet is formed by diamond particles and metal sintering, adopts common cored solder (as ormolu, copper silver kirsite etc.) to carry out soldering usually; Natural diamond and diamond and the common method of inlaying that adopts of combining of metal, and must carry out the metalized rear to diamond surface and can carry out soldering with common cored solder, shortcomings such as this method exists surface of the work pretreatment process and welding procedure complexity, and welding quality is restive.If directly carrying out soldering with common cored solder between diamond and the metal combines, because it is wetting by common cored solder that diamond surface is difficult to, do not have chemical reaction between diamond and the common cored solder, the combination between them only is a mechanical bond, does not reach the welding quality requirement far away.The welding quality of diamond and metal is a difficult problem always.
Summary of the invention
The object of the present invention is to provide a kind of diamond, ZrO of being directly used in 2The preparation method of the active solder of pottery and solder bonding metal solves diamond and metal in the prior art, ZrO 2The welding difficult problem of pottery and steel alloy.
The objective of the invention is to be achieved through the following technical solutions:
The alloy powder of A, powder metallurgic method is got the raw materials ready by following requirement and proportioning:
A, purity are 98~99%, granularity is the Ag of 40~45 μ m, and its percentage by weight ratio range is 49~69%;
B, purity are 98~99%, granularity is the Cu of 40~50 μ m, and its percentage by weight ratio range is 30~50%;
C, purity for>99%, granularity is the Ti of 20~25 μ m, its percentage by weight ratio range is 1~8%;
According to the soldering requirement, in above-mentioned scope, adjust the proportioning of three kinds of components;
B, compacting
With three kinds of powder by proportioning drop into common batch mixer dried be mixed even after, on the fast oil pressure machine, be pressed into block blank;
C, vacuum-sintering, annealing
The block blank that presses is packed in the vacuum induction heating furnace, be not less than 10 at 650~1000 ℃, vacuum -3Sintering is 0.5~1.5 hour under the Pa situation; Vacuum-sintering needs to carry out when charging into inert protective atmosphere to 2.5~3.5Pa; Blank behind the sintering was annealed 2~10 hours down at 600~700 ℃;
D, rolling
(a) blank after will annealing takes out from the vacuum induction heating furnace, and at hot mill rolling, the milling train temperature transfers to 550 ℃~650 ℃, and hot rolling---annealing---hot rolling is thinned to thin slice until blank for several times so repeatedly and is the thick soldering tablet of 1.2~1.8mm;
(b) cold rolling
The soldering tablet pickling that hot rolling is formed earlier, after washing the oxide-film on surface off, on cold-rolling mill, make thickness and be 0.12~0.18 superthin section, be fusing point at 780~830 ℃ Ag-Cu-Ti active solder, it is specially adapted to diamond cutter thick film and hard alloy cutter soldering, ZrO 2The soldering of pottery and steel alloy etc.
Owing to contain active element Ti in the scolder, and the solid solubility of Ti in the Ag-Cu alloy is very limited, and the proportion of Ti, fusing point and Ag-Cu alloy differ greatly, if adopt common smelting method for preparing Ag-Cu-Ti active solder will cause the solder compositions deviation because of low-melting component is volatile, cause gravity segregation because of each component proportion is different, cause rolling difficulty of processing to strengthen because of crystal grain is thick, and scolder is easily contaminated, so it is unworkable to prepare the Ag-Cu-Ti alloy with the method for common vacuum melting.The present invention adopts powder metallurgic method, and preparation Ag-Cu-Ti active solder has solved the problems referred to above.
The present invention compared with prior art has following outstanding advantage:
1, owing to contains active element Ti in the Ag-Cu-Ti active solder, therefore can significantly reduce the angle of wetting of diamond and cored solder, when this scolder is used for the soldering of diamond and metal, needn't carry out complicated metalized to diamond surface, and welding quality height, welding procedure is simple, can solve the problem such as diamond brazing complex process, welding quality instability of current existence.
2, creatively powder metallurgic method is applied to prepare the Ag-Cu-Ti active solder, not only technology is simple for it, economy, scolder purity height, and solved can not overcome in the smelting method for preparing such as the composition deviation, problems such as gravity segregation, the thick rolling difficulty of crystal grain.
3, be suitable for face width, can not only finish the soldering of diamond tool in high quality, and can be successfully used to the higher ZrO of difficulty 2The welding of pottery and metal etc.Simplified former welding procedure, and steady quality.
The specific embodiment
The present invention is described in further detail below by embodiment:
Embodiment 1:
The alloy powder of A, powder metallurgic method is got the raw materials ready by following requirement and proportioning:
Composition Purity (%) Granularity (μ m) Proportioning (wt%)
Ag 99 45 65
Cu 99 40 33
Ti 99.5 20 2
B, three kinds of alloy powders are dropped into common batch mixer do to mix 2 hours; Powder after mixing under the 550Mpa pressure, is pressed into block blank on THP-60A fast oil pressure machine.
C, pack the block blank that presses into the vacuum induction heating furnace common, suction to 10 -3Pa, and charge into Ar gas to 3Pa after vacuumizing was 700 ℃ of following sintering 1.2 hours.Blank behind the sintering was annealed 2 hours down at 650 ℃.
D, the blank after will annealing takes out from the vacuum induction heating furnace earlier, and at hot mill rolling, rolling temperature transfers to 600 ℃, and---annealing---hot rolling is repeatedly carried out repeatedly through hot rolling, is thinned to the thick soldering tablet of 1.5mm until blank; After the soldering tablet surface film oxide pickling after the hot rolling being fallen, be rolled into the active solder sheet material of 0.15mm on common cold, this sheet material fusing point is 780 ℃, successfully is applied to the soldering of CVD diamond thick-film in YG serial carbide alloy cutter again.
Embodiment 2:
The alloy powder of A, powder metallurgic method is got the raw materials ready by following requirement and proportioning:
Composition Purity (%) Granularity (μ m) Proportioning (wt%)
Ag 98 40 60
Cu 98 45 37
Ti 99 20 3
B, three kinds of alloy powders are dropped into common batch mixer do to mix 3 hours; Powder after mixing under the 500Mpa pressure, is pressed into block blank on THP-60A fast oil pressure machine.
C, pack the block blank that presses into the vacuum induction heating furnace common, suction to 10 -2Pa, and charge into Ar to 3.5Pa after vacuumizing was 750 ℃ of following sintering 1 hour.Blank behind the sintering was annealed 3 hours down at 650 ℃.
D, the blank after will annealing takes out from the vacuum induction heating furnace earlier, and in hot-rolling mill mechanism, rolling temperature transfers to 650 ℃, and---annealing---hot rolling is repeatedly carried out repeatedly through hot rolling, is thinned to the thick solder sheet of 1.8mm until blank; After the solder surface oxide-film pickling after the hot rolling being fallen, be rolled into the active solder sheet material of 0.18mm on common cold, this sheet material fusing point is 800 ℃, successfully is applied to the soldering of CVD diamond thick-film in YT serial carbide alloy cutter again.
Embodiment 3:
The alloy powder of A, powder metallurgic method is got the raw materials ready by following requirement and proportioning:
Composition Purity (%) Granularity (μ m) Proportioning (wt%)
Ag 99 50 60
Cu 99 45 34
Ti 99.9 25 6
B, three kinds of alloy powders are dropped into common batch mixer do to mix 4 hours; Powder after mixing under the 550Mpa pressure, is pressed into block blank on THP-60A fast oil pressure machine.
C, pack the block blank that presses into the vacuum induction heating furnace common, suction to 10 -3Pa, and charge into Ar gas to 2.5Pa after vacuumizing was 1000 ℃ of following sintering 0.8 hour.Blank behind the sintering was 700 ℃ of annealing 5 hours.
D, the blank after will annealing takes out from the vacuum induction heating furnace earlier, and in hot-rolling mill mechanism, rolling temperature transfers to 650 ℃, and---annealing---hot rolling is repeatedly carried out repeatedly through hot rolling, is thinned to the thick solder sheet of 1.2mm until blank; After the solder surface oxide-film pickling after the hot rolling being fallen, be rolled into the active solder sheet material of 0.12mm on common cold, this sheet material fusing point is 830 ℃, successfully is applied to ZrO again 2Pottery is in the soldering of 40Cr.

Claims (2)

1, a kind of preparation method of active solder is characterized in that adopting powder metallurgic method, through getting the raw materials ready, batch mixing, compacting, vacuum-sintering, annealing, hot rolling, cold-rolling process be prepared from the Ag-Cu-Ti active solder, its processing step is as follows:
A, get the raw materials ready by following requirement and proportioning:
A, purity are 98~99%, granularity is the Ag of 40~45 μ m, and its percentage by weight ratio range is 49~69%;
B, purity are 98~99%, granularity is the Cu of 40~50 μ m, and its percentage by weight ratio range is 30~50%;
C, purity for>99%, granularity is the Ti of 20~25 μ m, its percentage by weight ratio range is 1~8%;
B, compacting
With three kinds of powder by proportioning drop into common batch mixer dried be mixed even after, on the fast oil pressure machine, be pressed into block blank;
C, vacuum-sintering, annealing
The block blank that presses is packed in the vacuum induction heating furnace, and at 650~1000 ℃, vacuum was not less than under the 10-3Pa situation sintering 0.5~1.5 hour; Vacuum-sintering needs to carry out when charging into inert protective atmosphere to 2.5~3.5Pa; Blank behind the sintering was annealed 2~10 hours down at 600~700 ℃;
D, rolling
(a) hot rolling
Blank after the annealing is taken out, and at hot mill rolling, hot rolling---annealing---hot rolling is several so repeatedly, until the blank attenuate;
(b) cold rolling
Earlier hot rolling is formed the thick active soldering tablet pickling of 1.2~1.8mm, wash the oxide-film on surface off after, the active solder sheet material of making 0.12~0.18mm on cold-rolling mill is the Ag-Cu-Ti active solder.
2, the preparation method of a kind of active solder according to claim 1 is characterized in that the alloy powder composition of powder metallurgic method requires with proportioning as follows:
Purity is 99%, granularity is Ag and the Cu of 40 μ m, and Ag and Cu ratio are eutectic composition; Purity is 99.5%, granularity is the Ti of 20 μ m, its percentage by weight proportioning>1%.
CN99124681A 1999-12-27 1999-12-27 Active solder and its preparation Expired - Fee Related CN1094810C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN99124681A CN1094810C (en) 1999-12-27 1999-12-27 Active solder and its preparation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN99124681A CN1094810C (en) 1999-12-27 1999-12-27 Active solder and its preparation

Publications (2)

Publication Number Publication Date
CN1258580A CN1258580A (en) 2000-07-05
CN1094810C true CN1094810C (en) 2002-11-27

Family

ID=5283554

Family Applications (1)

Application Number Title Priority Date Filing Date
CN99124681A Expired - Fee Related CN1094810C (en) 1999-12-27 1999-12-27 Active solder and its preparation

Country Status (1)

Country Link
CN (1) CN1094810C (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100368140C (en) * 2004-06-03 2008-02-13 吉林大学 Method for connecting diamond thick film with hard base firmly
CN101012129B (en) * 2006-11-08 2010-04-14 吉林大学 Method of modifying diamond film or natural diamond surface
CN101913036A (en) * 2010-09-08 2010-12-15 郑州机械研究所 CuZnTi solder for soldering diamond tool
CN102699567A (en) * 2012-06-14 2012-10-03 中南大学 Zirconium-containing copper silver titanium solder alloy

Families Citing this family (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101333116B (en) * 2008-07-30 2010-06-02 哈尔滨工业大学 Method of Brazing ceramic and ceramic-based composite material with titan alloy
EP2469562A1 (en) * 2010-12-22 2012-06-27 ABB Technology AG Interrupter insert for a circuit breaker arrangement
CN102079000A (en) * 2011-02-14 2011-06-01 江阴东大新材料研究院 Ceramic for repairing damaged ceramic coating on surface of metal and argon arc welding method thereof
CN103084751A (en) * 2012-12-24 2013-05-08 镇江大有硬质材料有限公司 Diamond brazing welding flux
CN103170766A (en) * 2013-03-27 2013-06-26 江苏盛之祥电子科技有限公司 Preparation method of low-melting-point high-reliability lead-free solder
KR20160089429A (en) * 2013-11-22 2016-07-27 회가내스 아베 (피유비엘) Preforms for brazing
CN103752971A (en) * 2013-12-13 2014-04-30 天津大学 Method for connecting TC4 titanium alloy with silicon nitride ceramic by brazing connection with solders of titanium-silver-copper
CN104387103B (en) * 2014-11-19 2016-03-30 中国原子能科学研究院 The method for welding of a kind of zirconia ceramics and metallic substance
CN104387118B (en) * 2014-11-19 2016-05-04 中国原子能科学研究院 Zirconia ceramics metallization paste material formula, preparation method and application for a kind of soldering
CN105537799A (en) * 2015-12-24 2016-05-04 昆明贵金属研究所 Agcuti active brazing filler metal and preparation method thereof
CN107385439B (en) * 2017-06-02 2023-10-17 泉州众志金刚石工具有限公司 Cu-Ag-Ti diamond brazing coating and preparation method thereof
CN107309429B (en) * 2017-07-06 2019-05-21 北京理工大学 A kind of preparation method of powder accumulation structure all-metal active material
CN108103497B (en) * 2017-12-19 2020-10-27 东南大学 Method for preparing low-temperature welding titanium carbide coating
CN108085679A (en) * 2017-12-19 2018-05-29 东南大学 Low-temperature welding diamond coatings preparation method
CN109434317B (en) * 2018-11-16 2021-02-02 北京康普锡威科技有限公司 Lead-free environment-friendly solder and preparation method and application thereof
CN110394521B (en) * 2019-08-02 2021-03-23 太原理工大学 Diamond film high-efficiency heat dissipation material and preparation method thereof
CN112059470A (en) * 2020-09-08 2020-12-11 中物院成都科学技术发展中心 Active brazing filler metal for brazing titanate microwave dielectric ceramic and metal and preparation method thereof
CN113084176B (en) * 2021-04-09 2023-08-18 武汉工程大学 Self-supporting diamond film/Cu composite heat sink material and preparation method thereof
CN113600957A (en) * 2021-08-12 2021-11-05 合肥工业大学 Composite interlayer and method for brazing boron carbide composite ceramic and titanium alloy
CN114473289A (en) * 2022-01-20 2022-05-13 浙江亚通焊材有限公司 AgCu-based brazing filler metal and method for brazing and connecting diamond and copper by using AgCu-based brazing filler metal
CN115922147A (en) * 2022-12-27 2023-04-07 云南大学 Is suitable for Al 2 O 3 High-strength active brazing filler metal for ceramic welding and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4678720A (en) * 1985-01-04 1987-07-07 Gte Laboratories Incorporated Silver-copper-titanium brazing alloy
JPH1129371A (en) * 1997-07-10 1999-02-02 Tokuyama Corp Brazing material and jointing between aluminum nitride and metal material
JPH11130555A (en) * 1997-10-28 1999-05-18 Kyocera Corp Brazing material for joining ceramic-copper

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4678720A (en) * 1985-01-04 1987-07-07 Gte Laboratories Incorporated Silver-copper-titanium brazing alloy
JPH1129371A (en) * 1997-07-10 1999-02-02 Tokuyama Corp Brazing material and jointing between aluminum nitride and metal material
JPH11130555A (en) * 1997-10-28 1999-05-18 Kyocera Corp Brazing material for joining ceramic-copper

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100368140C (en) * 2004-06-03 2008-02-13 吉林大学 Method for connecting diamond thick film with hard base firmly
CN101012129B (en) * 2006-11-08 2010-04-14 吉林大学 Method of modifying diamond film or natural diamond surface
CN101913036A (en) * 2010-09-08 2010-12-15 郑州机械研究所 CuZnTi solder for soldering diamond tool
CN102699567A (en) * 2012-06-14 2012-10-03 中南大学 Zirconium-containing copper silver titanium solder alloy

Also Published As

Publication number Publication date
CN1258580A (en) 2000-07-05

Similar Documents

Publication Publication Date Title
CN1094810C (en) Active solder and its preparation
CN104646852B (en) Pricker applies cream and its application
EP2860273A1 (en) Heat-resistant molybdenum alloy
EP1592823B1 (en) A method of manufacturing a sputter target
CN102069189A (en) Powder metallurgy method for preparing high-purity materials
EP2716402A1 (en) Active metal brazing material
CN113351879A (en) Preparation method for cold deformation and heat treatment reinforced additive manufacturing of Cu-Ni-Sn alloy
JP2002371301A (en) Tungsten sintered compact and manufacturing method therefor
JP7081394B2 (en) Sputtering target and manufacturing method of sputtering target
CN1027797C (en) Anti-oxidation active metallic soldering material for welding ceramics
CN110576275A (en) Laser brazing in-situ reaction AgCuTiZr brazing filler metal and preparation method thereof
CN107470625A (en) A kind of powder metallurgy process for preparing high-purity material
JPH07233434A (en) Corrosion resistant material and its production
JPH0564691B2 (en)
JP5886473B2 (en) Ti-Al alloy sputtering target
JP2590255B2 (en) Copper material with good bondability with ceramics
JP2003303787A (en) Nickel alloy sputtering target and its manufacturing method
JPS63256291A (en) Material for adhesion
Do Nascimento et al. Brazing Al2O3 to sintered Fe-Ni-Co alloys
EP0368126B1 (en) Silver-copper-aluminum-titanium brazing alloy
JP6969466B2 (en) A method for manufacturing a molded body for joining and a joining method using the molded body for joining obtained by this method.
US4777015A (en) Process for producing tungsten heavy alloy sheet using a metallic salt binder system
Su et al. Interfacial reactions of liquid Sn and Sn-3.5 Ag solders with Ag thick films
JPH0292872A (en) Bonding between ceramic material and copper material
JP3015009B1 (en) Titanium silicide target and method of manufacturing the same

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C06 Publication
PB01 Publication
C14 Grant of patent or utility model
GR01 Patent grant
C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee