CN102820153A - Preparation method of refined AgSnO2In2O3 (silver tin oxide - indium oxide) crystal grain - Google Patents
Preparation method of refined AgSnO2In2O3 (silver tin oxide - indium oxide) crystal grain Download PDFInfo
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- CN102820153A CN102820153A CN2012102975613A CN201210297561A CN102820153A CN 102820153 A CN102820153 A CN 102820153A CN 2012102975613 A CN2012102975613 A CN 2012102975613A CN 201210297561 A CN201210297561 A CN 201210297561A CN 102820153 A CN102820153 A CN 102820153A
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Abstract
The invention provides a preparation method of refined AgSnO2In2O3 (silver tin oxide - indium oxide) crystal grains, which comprises the following steps of: a) conducting water atomization on Ag (silver), Sn (tin) and In (indium) to obtain AgSnIn powder; 2) statically pressing the AgSnIn powder into an AgSnIn ingot; 3) squeezing the AgSnIn ingot into AgSnIn wires, drawing the AgSnIn wires to Phi being 1.0-2.0mm and then oxidizing the wires; and 4) thrusting, squeezing and drawing the oxidized wires into AgSnO2In2O3 wires. Compared with the traditional method of enabling Ag, Sn and In elements to form an alloy phase, casting the alloy phase into the AgSnIn ingot, squeezing the AgSnIn ingot into wires and finally and interiorly oxidizing the wires, the preparation method has the advantages that since the AgSnIn alloy powder is prepared, the oxygen content of the alloy powder is increased, then the AgSnIn alloy powder is pressed into the AgSnIn ingot, the oxygen content of the AgSnIn alloy wires obtained through squeezing is high, the number of dislocation positions is great, the oxidization energy barrier is reduced during interior oxidization, the oxidizing speed is accelerated, the refined crystal boundaries and crystal grains are formed, the specific surface area of oxides in a composite material is increased and the fusion welding resistance of the material is enhanced.
Description
Technical field
The invention belongs to the metal-base composites field, be specifically related to a kind of preparation method of refinement silver-tin oxide or indium oxide crystal grain.
Background technology
The silver-tin oxide or indium oxide electrical contact material is mainly used in the appliance switches such as relay, contactor, motor engine, switch.This kind material is one of environment-friendly materials of in low-voltage electrical apparatus, using always at present.Miniaturization development and the harsh requirement of the life requirements of electrical equipment and raising of Chinese People's Anti-Japanese Military and Political College's electric current or the like along with relay; Resistance fusion welding and the anti-scorching type of each material preparation producer in order to improve material; Each show his special prowess for everybody, and main manufacture methods has preparation methods such as preoxidation, interior oxidation, traditional powder mixing method and chemical method.The each have their own advantage of these methods, the interpolation kind of the silver-tin oxide or indium oxide material additive of traditional powder mixing method and chemical method preparation is unrestricted, but the compactness of the material of its preparation is not high, and oxide particle is thick, forms oxide buildup easily; Tradition internal oxidation crystal boundary is big, and barren district of oxide and enrichment region are obvious, occur the incomplete phenomenon of oxidation easily; The preoxidation distribution of material is even, but its processing difficulties, and hardness is high, in the contact in the riveted joint process easy of crack.
The resistance fusion welding that improves the silver-tin oxide or indium oxide electrical contact material at present generally all is through the different processes method, adds one or more different additives.Specifically have following several document to relate to foregoing: 1) application number is the disclosed preparation method of Chinese patent " Nano Silver tin oxide or indium oxide electrical contact and preparation method thereof " of CN02146696.3; 2) application number is the disclosed preparation method of Chinese patent " a kind of preparation method of silver-tin oxide or indium oxide electrical contact " of CN03114863.8; 3) Shanghai non-ferrous metal magazine 2007 3 interim disclosed " additive is to the research of the nanocrystalline electrical contact material performance of silver-tin oxide or indium oxide "; 4) application number is disclosed preparation method in the Chinese patent " process for refining of preparation method silver nickel electric contact material grains process for refining and silver-tin oxide or indium oxide electrical contact material " of CN201010558978.1.Above-mentioned document 1) and 3) mix TiO through chemical plating respectively
2, the method that rare earth element reaches grain refinement effect and coats granules of stannic oxide at silver ammino solution, these two kinds all belong to chemical method, and the prepared strength of materials of this method is low, and compactness is poor.Document 2) atomization (pre-oxidation) Preparation of material, the method different oxidation states materials exhibit different characteristics, Bing and oxide content was high, the processing performance is poor.Document 4) be through jumping-up and repeatedly extrusion process reach the purpose of crystal grain thinning, mainly be to come broken wild phase through the means of big physical methods such as distortion, the crystal grain that refinement strengthens.
Summary of the invention
The objective of the invention is provides a kind of preparation method of refinement silver-tin oxide or indium oxide crystal grain in order to overcome the shortcoming and defect that prior art exists; This preparation method carries out refinement to the tissue of silver-tin oxide or indium oxide composite material; Through increasing the dislocation of alloy material; Reduce the oxidation energy barrier in the oxidizing process, accelerated oxidation rate, made crystal boundary and grain refinement; Thereby improved the resistance fusion welding of silver-tin oxide or indium oxide electrical contact material, improved its electrical property; Reducing simultaneously effectively silver assembles and defective such as separates out.
The present invention realizes through following technical scheme:
A kind of preparation method of refinement silver-tin oxide or indium oxide crystal grain is characterized in that, may further comprise the steps:
(1) Ag, Sn and In are carried out water atomization, obtain the AgSnIn powder; The weight content of Ag is 86%-95% in the said AgSnIn powder, and the weight content of In is 1.5%-6%, and surplus is Sn;
(2) the AgSnIn powder is pressed into the AgSnIn ingot through waiting static pressure;
(3) the AgSnIn ingot is squeezed into AgSnIn silk material, is drawn to
and carries out a material oxidation then;
(4) the silk material after the oxidation is thrust, pushes, is drawn into AgSnO
2In
2O
3The silk material.
Further setting of the present invention is that the hydraulic pressure that water atomization is adopted in the described step (1) is 30Mpa-40Mpa.
Further setting of the present invention is that the particle mean size of AgSnIn powder is 3 μ m-16 μ m in the step (1).
Further setting of the present invention is that the hydrostatic pressure in the described step (2) is 100Mpa-180Mpa, and the dwell time is 5s-30s, and the spindle diameter dimension is 80cm-108cm.
Further setting of the present invention is that said step (3) comprises following substep:
(a) with the AgSnIn ingot be squeezed into diameter
the silk material;
(b) the silk material is drawn to
(c) the silk material is stacked oxidation on the bin, the oxidation technology parameter is: oxygen is pressed 0.6MPa-2MPa, and 500 ℃-600 ℃ of oxidizing temperatures oxidation 1-2 hour, rise to 650 ℃-800 ℃, oxidation 20-30 hour.
Further setting of the present invention is that said step (4) comprises following substep:
(A) thrust to 15mm-30mm the silk material after the oxidation long;
(B) under air atmosphere after the heat treatment; Be pressed into ingot blank with hydraulic press, ingot blank carried out 1-2 multiple the pressure obtain
(C), be squeezed into the silk material of diameter for
corresponding specification of drawing 800 ℃ of-900 ℃ of sintering temperatures 3 hours-4 hours.
With in the past with Sn three kinds of elements form alloy phases and be cast into the AgSnIn ingot, be squeezed into a material, oxidation is compared in carrying out then; The preparation method of refinement silver-tin oxide or indium oxide crystal grain of the present invention through being prepared into the AgSnIn alloyed powder, increases the oxygen content of alloyed powder; Be pressed into the AgSnIn ingot again, the AgSnIn alloy silk oxygen content that is squeezed into is many, and dislocation is many; Thereby when interior oxidation, the oxidation energy barrier reduces, thus accelerated oxidation speed has formed refinement crystal boundary and crystal grain; Increase the oxide specific area of composite material, the resistance fusion welding of reinforcing material.
Description of drawings
Fig. 1 is a preparation method's according to the invention process chart;
Fig. 2 is the metallograph after the oxidation of employing internal oxidation process among the embodiment one;
Fig. 3 is the metallograph after embodiment one adopts technology oxidation of the present invention;
Fig. 4 is the metallograph after the oxidation of employing internal oxidation process among the embodiment two;
Fig. 5 is the metallograph after embodiment two adopts technology oxidation of the present invention.
Embodiment
Below in conjunction with Fig. 1 and embodiment the present invention is carried out concrete description; Only be used for the present invention is further specified; Can not be interpreted as the qualification to protection range of the present invention, the technician in this field can make some nonessential improvement and adjustment to the present invention according to the content of foregoing invention.
Embodiment one:
Silver plate with 99.99%, 99.5% Sn ingot, 99.97% In ingot is by than row 86:8:6; Alloying in intermediate frequency furnace is crossed 300 mesh sieves after the hydraulic pressure of 30MPa is atomized into the AgSn alloyed powder, and screenings is with 100Ma pressurize 30s in isostatic pressing machine; Obtain the spindle of diameter 95mm-105mm, in diameter is the recipient of 110mm, be squeezed into the AgSnIn alloy wire that diameter is 5mm, after being drawn to diameter and being 1.2mm; In the oxidation technology parameter is 500 ℃, and oxidation 1 hour rises to 650 ℃; Oxidation 30 hours, omnidistance oxygen are pressed and are 2Mpa; After judging port oxidation fully; It is long to thrust 15mm-30mm again; Under air atmosphere after the heat treatment; Be pressed into ingot blank with hydraulic press; Ingot blank is carried out 1-2 multiple the pressure obtain 85mm-108mm,, be squeezed into diameter and be
drawing 1.38 800 ℃ of-900 ℃ of sintering temperatures 3 hours-4 hours.
After table 1 is prepared into the finished silk material, the contrast of the physical property of two kinds of technologies
Material physical property from table 1, the volume resistance of material has decline.Because oxide particle is tiny, the performance ratio is the hardness and the tensile strength height of interior oxidation metallization processes in the past, but good percentage elongation, the visible material working plasticity more has improvement.Behind the simultaneous oxidation thing wild phase grain refine, increased the surface area of oxide, and oxide is evenly fine in silver matrix, material thermal resistance can be improved, thereby improved the resistance fusion welding of material.Fig. 2 is a metallograph after the oxidation of employing internal oxidation process, and visible its crystal boundary is few, and oxide particle is thick; Fig. 3 is the metallograph after the technology oxidation of adopting in the present embodiment, and visible its crystal boundary is many, and oxide particle is tiny.
Embodiment two:
Silver plate with 99.99%, 99.5% Sn ingot, 99.97% In ingot is by than row 95:3.5:1.5; Alloying in intermediate frequency furnace is crossed 300 mesh sieves (average grain is 12) after the hydraulic pressure of 30MPa is atomized into the AgSnIn alloyed powder, and screenings is with 100Ma pressurize 30s in isostatic pressing machine; Obtaining the spindle of diameter 95mm-105mm, is that the diameter that is squeezed into of 110mm is the 5mmAgSnIn alloy wire at diameter, after being drawn to diameter and being 1.2mm; In the oxidation technology parameter is 600 ℃, and oxidation 2 hours rises to 800 ℃; Oxidation 20 hours, omnidistance oxygen is pressed 0.6MPa; After judging port oxidation fully; It is long to thrust 15mm-30mm again; Under air atmosphere after the heat treatment; Be pressed into ingot blank with hydraulic press; Ingot blank is carried out 1-2 multiple the pressure obtain 85mm-108mm,, be squeezed into diameter and be
drawing 1.38 800 ℃ of-900 ℃ of sintering temperatures 3 hours-4 hours.
After table 2 is prepared into the finished silk material, the contrast of the physical property of two kinds of technologies
Material physical property from table 2, the volume resistance of material has decline, because oxide particle is tiny; The performance ratio is the hardness and the tensile strength height of interior oxidation metallization processes in the past, but good percentage elongation, therefore; Behind the oxide wild phase grain refine, increase the surface area of oxide, improved the resistance fusion welding of material; But from good elongation, drawing abillity can not reduce.Fig. 4 is a metallograph after the oxidation of employing internal oxidation process, and visible its crystal boundary is few, and oxide particle is thick; Fig. 5 is the metallograph after the technology oxidation of adopting in the present embodiment, and visible its crystal boundary is many, and oxide particle is tiny.
Claims (6)
1. the preparation method of a refinement silver-tin oxide or indium oxide crystal grain is characterized in that, may further comprise the steps:
(1) Ag, Sn and In are carried out water atomization, obtain the AgSnIn powder; The weight content of Ag is 86%-95% in the said AgSnIn powder, and the weight content of In is 1.5%-6%, and surplus is Sn;
(2) the AgSnIn powder is pressed into the AgSnIn ingot through waiting static pressure;
(3) the AgSnIn ingot is squeezed into AgSnIn silk material, is drawn to
and carries out a material oxidation then;
(4) the silk material after the oxidation is thrust, pushes, is drawn into AgSnO
2In
2O
3The silk material.
2. the preparation method of a kind of refinement silver-tin oxide or indium oxide crystal grain according to claim 1 is characterized in that: the hydraulic pressure that water atomization is adopted in the described step (1) is 30Mpa-40Mpa.
3. the preparation method of a kind of refinement silver-tin oxide or indium oxide crystal grain according to claim 1 is characterized in that: the particle mean size of AgSnIn powder is 3 μ m-16 μ m in the step (1).
4. a kind of refinement silver-tin oxide or indium oxide grain preparation method according to claim 1,, it is characterized in that: the hydrostatic pressure in the described step (2) is 100Mpa-180Mpa, and the dwell time is 5s-30s, and the spindle diameter dimension is 80cm-108cm.
5. a kind of refinement silver-tin oxide or indium oxide crystal grain preparation method according to claim 1, it is characterized in that: said step (3) comprises following substep:
(a) with the AgSnIn ingot be squeezed into diameter
the silk material;
(b) the silk material is drawn to
(c) the silk material is stacked oxidation on the bin, the oxidation technology parameter is: oxygen is pressed 0.6-2MPa, and 500 ℃-600 ℃ of oxidizing temperatures oxidation 1-2 hour, rise to 650 ℃-800 ℃, oxidation 20 hours-30 hours.
6. a kind of refinement silver-tin oxide or indium oxide crystal grain preparation method according to claim 1, it is characterized in that: said step (4) comprises following substep:
(A) thrust to 15mm-30mm the silk material after the oxidation long;
(B) under air atmosphere after the heat treatment; Be pressed into ingot blank with hydraulic press, ingot blank carried out 1-2 multiple the pressure obtain
(C), be squeezed into the silk material of diameter for
corresponding specification of drawing 800 ℃ of-900 ℃ of sintering temperatures 3 hours-4 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105349818A (en) * | 2015-11-20 | 2016-02-24 | 温州宏丰电工合金股份有限公司 | Oxide local graded distribution type electric contact material and preparation method thereof |
| CN105702503A (en) * | 2016-04-11 | 2016-06-22 | 福达合金材料股份有限公司 | Preparation method for silver tin oxide indium oxide contact material |
| CN110423908A (en) * | 2019-08-23 | 2019-11-08 | 温州宏丰电工合金股份有限公司 | One kind can quickly aoxidize silver-tin oxide or indium oxide contact material and preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5446110A (en) * | 1977-09-20 | 1979-04-11 | Sumitomo Electric Ind Ltd | Material for electrical contact point material and its preparation |
| CN101608279A (en) * | 2009-07-20 | 2009-12-23 | 温州宏丰电工合金有限公司 | Silver oxide electrical contact material and preparation method thereof |
| CN102031438A (en) * | 2010-12-31 | 2011-04-27 | 桂林电器科学研究院 | Sliver stannic oxide electrical contact material and preparation method thereof |
| CN102154572A (en) * | 2011-05-25 | 2011-08-17 | 宁波汉博贵金属合金有限公司 | Method for preparing sliver-tin oxide and indium oxide electrical contact material by gradient internal oxidation method and material thereof |
| CN102312119A (en) * | 2010-06-29 | 2012-01-11 | 福达合金材料股份有限公司 | Preparation method for silver tin oxide electrical contact material |
-
2012
- 2012-08-21 CN CN2012102975613A patent/CN102820153A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5446110A (en) * | 1977-09-20 | 1979-04-11 | Sumitomo Electric Ind Ltd | Material for electrical contact point material and its preparation |
| CN101608279A (en) * | 2009-07-20 | 2009-12-23 | 温州宏丰电工合金有限公司 | Silver oxide electrical contact material and preparation method thereof |
| CN102312119A (en) * | 2010-06-29 | 2012-01-11 | 福达合金材料股份有限公司 | Preparation method for silver tin oxide electrical contact material |
| CN102031438A (en) * | 2010-12-31 | 2011-04-27 | 桂林电器科学研究院 | Sliver stannic oxide electrical contact material and preparation method thereof |
| CN102154572A (en) * | 2011-05-25 | 2011-08-17 | 宁波汉博贵金属合金有限公司 | Method for preparing sliver-tin oxide and indium oxide electrical contact material by gradient internal oxidation method and material thereof |
Non-Patent Citations (1)
| Title |
|---|
| AMITABH VERMA等: "银氧化锡氧化铟电触头材料的加工及其特性", 《电工材料》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105349818A (en) * | 2015-11-20 | 2016-02-24 | 温州宏丰电工合金股份有限公司 | Oxide local graded distribution type electric contact material and preparation method thereof |
| CN105349818B (en) * | 2015-11-20 | 2017-07-11 | 温州宏丰电工合金股份有限公司 | A kind of contact material of oxide partial gradient distribution and preparation method thereof |
| CN105702503A (en) * | 2016-04-11 | 2016-06-22 | 福达合金材料股份有限公司 | Preparation method for silver tin oxide indium oxide contact material |
| CN110423908A (en) * | 2019-08-23 | 2019-11-08 | 温州宏丰电工合金股份有限公司 | One kind can quickly aoxidize silver-tin oxide or indium oxide contact material and preparation method |
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Application publication date: 20121212 |