CN108044259A - A kind of preparation method of stop-off gent for stainless-steel vacuum soldering - Google Patents

A kind of preparation method of stop-off gent for stainless-steel vacuum soldering Download PDF

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Publication number
CN108044259A
CN108044259A CN201711245418.9A CN201711245418A CN108044259A CN 108044259 A CN108044259 A CN 108044259A CN 201711245418 A CN201711245418 A CN 201711245418A CN 108044259 A CN108044259 A CN 108044259A
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China
Prior art keywords
mixture
powder
gent
stop
added
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CN201711245418.9A
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CN108044259B (en
Inventor
蔡伟炜
沈涛
张继
祁更新
陈晓
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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Wenzhou Hongfeng Electrical Alloy Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3601Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
    • B23K35/361Alumina or aluminates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/362Selection of compositions of fluxes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K37/00Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups
    • B23K37/06Auxiliary devices or processes, not specially adapted to a procedure covered by only one of the preceding main groups for positioning the molten material, e.g. confining it to a desired area

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to welding technology fields, it is desirable to provide a kind of preparation method of stop-off gent for stainless-steel vacuum soldering.Including:After Zirconium powder, titanium oxide powder ball milling, mixture one is obtained;Mixture two will be obtained after mixture one and alumina powder, neodymia powder ball milling;Propylene glycol is added in into VAE lotions with deionized water after mixing and is stirred evenly, obtains mixture three;Mixture four is obtained after methylcellulose and Acritamer 940 stirring are added in into mixture three;Mixture two is added in mixture four after stirring and obtain mixture five;Ammonium hydroxide is added in into mixture five while stirring and adjusts pH to 8~10, after then grinding, obtains the stop-off gent for stainless-steel vacuum soldering.The present invention solves the problems, such as that oxide component occurs sintering and forms hard aggregation or caking in stop-off gent in the process of stainless-steel vacuum soldering, can be removed it after soldering by the non-destructive modes such as wash, blow, not disfiguring workpiece surface.

Description

A kind of preparation method of stop-off gent for stainless-steel vacuum soldering
Technical field
The present invention relates to welding technology fields, and in particular to a kind of preparation side of stop-off gent for stainless-steel vacuum soldering Method.
Background technology
Stop-off gent is to be used for protecting by a kind of material of weldering metal surface in brazing process, is by oxide and bonding Agent mixes and stable suspension system is made, and can be configured to have suitable viscosity and rheology spy according to the difference for applying technique Property composition, the solder of melting can effectively be prevented arbitrarily to trickle being brazed metal surface under brazing temperature, it is required It is to remove in a certain way after brazing, without polluting and corroding metal works.
The brazing temperature of nickel-based solder is higher used in stainless-steel vacuum soldering, generally at 1000 DEG C or so, and commonly uses at present Stop-off gent oxide filler include aluminium oxide, chromium oxide, titanium oxide, magnesia etc., under this hot conditions, conventional stop-off gent Including aluminium oxide, chromium oxide, titanium oxide, magnesia etc. different degrees of sintering can occur for oxide used, and be formed hard Reunion or caking phenomenon hinder so as to cause that can not pass through non-demolition mode (such as washing, air blowing, solvent are washed) removal after brazing Flow agent residual.And remained by the destructive means such as polishing, polishing although stop-off gent can be effectively removed, also workpiece surface is made Into permanent damage.Therefore, the stop-off gent for stainless-steel vacuum soldering after should having vacuum brazing remains, reunites less, few less The characteristics of scleroma, easy-clear.
The content of the invention
The technical problem to be solved by the present invention is to overcome deficiency of the prior art, provide a kind of for stainless-steel vacuum The preparation method of the stop-off gent of soldering.
To solve technical problem, solution of the invention is:
A kind of preparation method of the stop-off gent for stainless-steel vacuum soldering is provided, is included the following steps:
(1) each component is weighed by weight percentage:Zirconium powder 5%-10%;Titanium oxide powder 5%-10%;Oxidation Aluminium powder body 35%-55%;Neodymia powder 0.5%-5%;Acritamer 940:0.15%-0.5%;VAE lotions 4.0%- 9.0%;Methylcellulose 1.5%-5%;Propylene glycol 2%-4%;Deionized water 18%-30.35%;
(2) Zirconium powder, titanium oxide powder are added in ball grinder, when ball milling 6~12 is small, is taken after being cooled to room temperature Go out, obtain mixture one;
(3) mixture one and alumina powder, neodymia powder are added in ball grinder together, when ball milling 24~36 is small, It is taken out after being cooled to room temperature, obtains mixture two;
(4) propylene glycol with deionized water is mixed, after stirring evenly, adds in VAE lotions and stir evenly, obtain mixture Three;
(5) methylcellulose and Acritamer 940 are added in into mixture three, and is warming up to 65~85 DEG C, stirring 30~60 Minute, after being cooled to room temperature, obtain mixture four;
(6) mixture two is added in mixture four, when stirring 1~3 is small, mixture five is obtained after being cooled to room temperature;
(7) ammonium hydroxide is added in into mixture five while stirring, pH to 8~10 is adjusted, is then ground using three-roll grinder 10~25 times, after being cooled to room temperature, obtain the stop-off gent for stainless-steel vacuum soldering.
In the present invention, the grain size of the Zirconium powder is between 10~50 microns.
In the present invention, the grain size of the titanium oxide powder is between 5~25 microns;
In the present invention, the grain size of the alumina powder is between 10~50 microns;
In the present invention, the grain size of the neodymia powder is between 1~10 micron;
In the present invention, the VAE lotions be in GW-705 or GW-707 type products (production of Guangxi Guang Wei companies) extremely Few one kind.
The realization principle of the present invention:
1st, by many experiments filter out rare earth oxide neodymia (at high temperature, neodymia with good pinning make With the sintering of oxide powder can be inhibited) with zirconium oxide cooperation as improvement stop-off gent hard aggregation or the raw material of agglomeration problems, And pass through the optimum combination that testing sieve selects neodymia and zirconium oxide, it solves oxide component in stop-off gent and occurs to be sintered and shape The problem of into hard aggregation or caking, asks in addition, neodymia or zirconium oxide is used alone as improvement stop-off gent hard aggregation or caking It is ineffective during the raw material of topic.
2nd, since this stop-off gent is not sintered after vacuum brazing, with stainless steel work-piece oxide on surface and It is combined without apparent, stop-off gent provided by the invention can be gone after for vacuum brazing by the non-destructive modes such as wash, blow Removal of residue.
Compared with prior art, the invention has the advantages that:
The present invention provides a kind of stop-off gent for titanium alloy vacuum brazing, solves the processing in stainless-steel vacuum soldering The problem of oxide component occurs sintering and forms hard aggregation or caking in stop-off gent in the process, can be by washing, blowing after soldering The non-destructive modes such as gas remove it, not disfiguring workpiece surface.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this field For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection domain.
Embodiment 1:
The present invention provide it is a kind of for stainless-steel vacuum soldering stop-off gent, it is characterised in that by following weight content into It is grouped into
Zirconium powder:5%
Titanium oxide powder:10%
Alumina powder:35%
Neodymia powder:5%
Acritamer 940:0.15%
VAE lotions:9.0%
Methylcellulose:1.5%
Propylene glycol:4%
Deionized water:30.35%
The grain size of the Zirconium powder is between 10 microns~25 microns, and the grain size of titanium oxide powder is 15 microns~25 Between micron, the grain size of alumina powder is between 10 microns~25 microns, and the grain size of neodymia powder is at 6 microns~10 microns Between;VAE lotions are the GW-705 that Guangxi is extensively tieed up.
The preparation method of above-mentioned stop-off gent, includes the following steps:
(1) each component is weighed by the weight percent;
(2) Zirconium powder, titanium oxide powder are added in ball grinder, when ball milling 6 is small, takes out, obtain after being cooled to room temperature To mixture one;
(2) alumina powder and neodymia powder are added in mixture one, and added in together in ball grinder, ball milling 36 it is small when, removed after being cooled to room temperature, obtain mixture two;
(2) after being mixed and stirred for propylene glycol and deionized water uniformly, VAE lotions is added in and are stirred evenly, obtain mixture Three;
(2) methylcellulose and Acritamer 940 are added in into mixture three, and is warming up to 65 DEG C, it is cold when stirring 1 is small But to obtaining mixture four after room temperature;
(2) mixture two is added in mixture four, when stirring 1 is small, mixture five is obtained after being cooled to room temperature;
(2) ammonium hydroxide is added in into mixture five while stirring, adjusts PH to 10, then grinds 10 using three-roll grinder It is secondary, the stop-off gent for stainless-steel vacuum soldering is obtained after being cooled to room temperature.
Embodiment 2:
The present invention provide it is a kind of for stainless-steel vacuum soldering stop-off gent, it is characterised in that by following weight content into It is grouped into
Zirconium powder:10%
Titanium oxide powder:5%
Alumina powder:55%
Neodymia powder:0.5%
Acritamer 940:0.5%
VAE lotions:4.0%
Methylcellulose:5%
Propylene glycol:2%
Deionized water:18%
The grain size of the Zirconium powder is between 25 microns~50 microns, and the grain size of titanium oxide powder is 5 microns~15 Between micron, the grain size of alumina powder is between 25 microns~50 microns, and the grain size of neodymia powder is at 1 micron~6 microns Between, VAE lotions are the GW-707 that Guangxi is extensively tieed up.
The preparation method of above-mentioned stop-off gent, includes the following steps:
(1) each component is weighed by the weight percent;
(2) Zirconium powder, titanium oxide powder are added in ball grinder, when ball milling 12 is small, takes out, obtain after being cooled to room temperature To mixture one;
(2) alumina powder and neodymia powder are added in mixture one, and added in together in ball grinder, ball milling 24 it is small when, removed after being cooled to room temperature, obtain mixture two;
(2) after being mixed and stirred for propylene glycol and deionized water uniformly, VAE lotions is added in and are stirred evenly, obtain mixture Three;
(2) methylcellulose and Acritamer 940 are added in into mixture three, and is warming up to 85 DEG C, is stirred 30 minutes, it is cold But to obtaining mixture four after room temperature;
(2) mixture two is added in mixture four, when stirring 3 is small, mixture five is obtained after being cooled to room temperature;
(2) ammonium hydroxide is added in into mixture five while stirring, adjusts PH to 8, is then ground 25 times using three-roll grinder, The stop-off gent for stainless-steel vacuum soldering is obtained after being cooled to room temperature.
Embodiment 3:
The present invention provide it is a kind of for stainless-steel vacuum soldering stop-off gent, it is characterised in that by following weight content into It is grouped into
Zirconium powder:7.5%
Titanium oxide powder:7.5%
Alumina powder:45%
Neodymia powder:3%
Acritamer 940:0.35%
VAE lotions:6.5%
Methylcellulose:3.5%
Propylene glycol:3%
Deionized water:23.65%
The grain size of the Zirconium powder is between 15 microns~35 microns, and the grain size of titanium oxide powder is 10 microns~20 Between micron, the grain size of alumina powder is between 15 microns~35 microns, and the grain size of neodymia powder is at 3 microns~7 microns Between, VAE lotions are the GW-705 that Guangxi is extensively tieed up and GW-707 with mass ratio 1:1 mixing.
The preparation method of above-mentioned stop-off gent, includes the following steps:
(1) each component is weighed by the weight percent;
(2) Zirconium powder, titanium oxide powder are added in ball grinder, when ball milling 9 is small, takes out, obtain after being cooled to room temperature To mixture one;
(2) alumina powder and neodymia powder are added in mixture one, and added in together in ball grinder, ball milling 30 it is small when, removed after being cooled to room temperature, obtain mixture two;
(2) after being mixed and stirred for propylene glycol and deionized water uniformly, VAE lotions is added in and are stirred evenly, obtain mixture Three;
(2) methylcellulose and Acritamer 940 are added in into mixture three, and is warming up to 75 DEG C, is stirred 45 minutes, it is cold But to obtaining mixture four after room temperature;
(2) mixture two is added in mixture four, when stirring 2 is small, mixture five is obtained after being cooled to room temperature;
(2) ammonium hydroxide is added in into mixture five while stirring, adjusts PH to 9, is then ground 18 times using three-roll grinder, The stop-off gent for stainless-steel vacuum soldering is obtained after being cooled to room temperature.
Invention effect is verified
1st, the stop-off gent for stainless-steel vacuum soldering that embodiment 1 is prepared, is denoted as sample one.
2nd, the stop-off gent that commercially available product type is Nicrobraz White Stop Off (wall colmonoy) is taken, It is denoted as sample two.
3rd, by the above-mentioned two of acquisition for stainless-steel vacuum soldering stop-off gent product coated on 304 stainless steel surfaces into Row vacuum brazing, used after soldering blow mode (gas flow rate is 3 × 105Pa, incident angle be 90 °, nozzle away from coated with The surface 200mm of stop-off gent) removal 304 stainless steel surfaces stop-off gent residual, measuring its surface gloss, (glossiness is included in Firing angle is 60 °) to characterize stop-off gent residual condition (residual more at most gloss value lower), test result such as following table institute Show.
Sample Glossiness
Sample one 580
Sample two 230
By upper table as can be seen that compared with stop-off gent of the prior art, stop-off gent using the present invention can effectively be kept away Exempt from oxide component in stop-off gent sintering occurs and forms hard aggregation or caking, and stop-off gent is caused to be difficult to after vacuum brazing It removes, stop-off gent of the invention can go removal of residue, technology after for soldering by the non-destructive modes such as wash, blow In contrast effect is very significant.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring the substantive content of the present invention.

Claims (6)

1. the preparation method of a kind of stop-off gent for stainless-steel vacuum soldering, which is characterized in that include the following steps:
(1) each component is weighed by weight percentage:Zirconium powder 5%-10%;Titanium oxide powder 5%-10%;Alumina powder Body 35%-55%;Neodymia powder 0.5%-5%;Acritamer 940:0.15%-0.5%;VAE lotions 4.0%-9.0%;First Base cellulose 1.5%-5%;Propylene glycol 2%-4%;Deionized water 18%-30.35%;
(2) Zirconium powder, titanium oxide powder are added in ball grinder, when ball milling 6~12 is small, takes out, obtain after being cooled to room temperature To mixture one;
(3) mixture one and alumina powder, neodymia powder are added in ball grinder together, when ball milling 24~36 is small, cooling It is taken out after to room temperature, obtains mixture two;
(4) propylene glycol with deionized water is mixed, after stirring evenly, adds in VAE lotions and stir evenly, obtain mixture three;
(5) methylcellulose and Acritamer 940 are added in into mixture three, and is warming up to 65~85 DEG C, is stirred 30~60 minutes, After being cooled to room temperature, mixture four is obtained;
(6) mixture two is added in mixture four, when stirring 1~3 is small, mixture five is obtained after being cooled to room temperature;
(7) add in ammonium hydroxide into mixture five while stirring, adjust pH to 8~10, then using three-roll grinder grinding 10~ 25 times, after being cooled to room temperature, obtain the stop-off gent for stainless-steel vacuum soldering.
2. according to the method described in claim 1, it is characterized in that, the grain size of the Zirconium powder 10~50 microns it Between.
3. the method according to claim 1, which is characterized in that the grain size of the titanium oxide powder is between 5~25 microns.
4. the method according to claim 1, which is characterized in that the grain size of the alumina powder is between 10~50 microns.
5. the method according to claim 1, which is characterized in that the grain size of the neodymia powder is between 1~10 micron.
6. the method according to claim 1, which is characterized in that the VAE lotions are in GW-705 or GW-707 type products It is at least one.
CN201711245418.9A 2017-12-01 2017-12-01 Preparation method of flow resisting agent for stainless steel vacuum brazing Active CN108044259B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110732806A (en) * 2018-07-20 2020-01-31 千住金属工业株式会社 Soldering flux and solder paste
CN111482728A (en) * 2020-04-17 2020-08-04 中车青岛四方机车车辆股份有限公司 Flow resisting agent for brazing and preparation method thereof

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US3906617A (en) * 1970-03-04 1975-09-23 Gte Sylvania Inc Method of preventing braze and diffusion flow
JPS59133991A (en) * 1983-01-21 1984-08-01 Honda Motor Co Ltd Film for preventing sticking of welding spatter
CN102182907A (en) * 2010-12-06 2011-09-14 中国航空工业集团公司北京航空制造工程研究所 Titanium alloy I-shaped section corrugation girder and manufacturing method thereof
CN102500907A (en) * 2011-10-26 2012-06-20 首都航天机械公司 Method for precise control of diffusion welding / stop welding region
CN102807374A (en) * 2012-07-12 2012-12-05 中国电子科技集团公司第五十五研究所 Solder resist for high-temperature co-fired multilayer ceramic and preparation method of solder resist
CN103579136A (en) * 2012-07-30 2014-02-12 通用电气公司 Diffusion barrier for surface-mount modules
CN107009090A (en) * 2016-01-27 2017-08-04 鞍钢股份有限公司 Production method of stainless steel composite board

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3906617A (en) * 1970-03-04 1975-09-23 Gte Sylvania Inc Method of preventing braze and diffusion flow
JPS59133991A (en) * 1983-01-21 1984-08-01 Honda Motor Co Ltd Film for preventing sticking of welding spatter
CN102182907A (en) * 2010-12-06 2011-09-14 中国航空工业集团公司北京航空制造工程研究所 Titanium alloy I-shaped section corrugation girder and manufacturing method thereof
CN102500907A (en) * 2011-10-26 2012-06-20 首都航天机械公司 Method for precise control of diffusion welding / stop welding region
CN102807374A (en) * 2012-07-12 2012-12-05 中国电子科技集团公司第五十五研究所 Solder resist for high-temperature co-fired multilayer ceramic and preparation method of solder resist
CN103579136A (en) * 2012-07-30 2014-02-12 通用电气公司 Diffusion barrier for surface-mount modules
CN107009090A (en) * 2016-01-27 2017-08-04 鞍钢股份有限公司 Production method of stainless steel composite board

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110732806A (en) * 2018-07-20 2020-01-31 千住金属工业株式会社 Soldering flux and solder paste
CN111482728A (en) * 2020-04-17 2020-08-04 中车青岛四方机车车辆股份有限公司 Flow resisting agent for brazing and preparation method thereof

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