CN115466873A - Base metal ion doped modified silver tin oxide material and preparation method and application thereof - Google Patents
Base metal ion doped modified silver tin oxide material and preparation method and application thereof Download PDFInfo
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
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Abstract
The invention discloses a preparation method of a base metal ion doped modified silver tin oxide material. The problem that the service life of the electric contact is short due to poor wettability between tin oxide and a silver matrix in the preparation of the existing silver tin oxide electric contact material is solved. The method comprises the following steps: preparing base metal doped tin oxide powder by a self-propagating combustion method and a high-temperature solid phase method, and mixing the base metal ion doped tin oxide powder with silver powder to obtain mixed powder; primarily pressing the mixed powder to obtain a blank; primarily sintering the blank to obtain a sintered blank; re-pressing the sintered blank; and (7) re-burning. The doping of the basic metal ions can improve the wettability between tin oxide and a silver matrix; the high-energy ball milling mixed powder is combined to ensure the high-efficiency densification of the material, improve the dispersion effect of the second phase and improve the electrical contact performance. The method is suitable for preparing the silver tin oxide electric contact material.
Description
Technical Field
The invention relates to the field of base metal doped materials, in particular to a base metal ion doped modified silver tin oxide material and a preparation method and application thereof.
Background
The contact element of the low-voltage electrical appliance is made of silver-based electric contact materials manufactured by a powder metallurgy method. The low-voltage electric contact element is in service under the alternating load conditions of mechanical impact, partial arc ablation and the like, so that high requirements are put forward on the arc ablation resistance of the electric contact material. Among electrical contact materials for contactors, ag/CdO has the most excellent performance and is widely used in various application levels. However, since Cd has a serious toxicity, the european union issued RoHS directive in 2002, and the use of Cd in electronic and electric appliances was definitely prohibited.
For many years, researchers have found that specific oxides, such as In, can be added 2 O 3 CuO, can effectively improve Ag and SnO 2 Thereby improving the electrical life of the electrical contact. Subsequently, researchers hypothesized that the addition of oxides could increase Ag and SnO 2 The key to the wettability of (A) is that Cu from CuO is under the action of an electric arc 2+ Doped into SnO 2 The crystal lattice of (2) changes the physicochemical properties thereof, thereby enabling the crystal lattice to have better wettability with Ag. Based on this hypothesis, researchers have conducted a large number of different base metal ion-doped modified SnO 2 Investigation of/Ag electrical contact materials, e.g. Cu 2+ ,Fe 3+ ,Al 3+ ,Sb 5+ Etc.), the results show that the doping of the basic metal ions can effectively improve Ag and SnO 2 Thereby extending the electrical life of the electrical contact. However, on the one hand, because the ablation conditions of the research are not uniform, the doped base metal ions for prolonging the electrical life of the electrical contact optimally are not determined; on the other hand, doped SnO 2 The preparation process of the powder has the problems of high cost, environmental pollution, low yield and the like.
Through years of research, ag/SnO 2 The contact material is considered to be the best alternative. But according to 2020 electric industry in ChinaThe industry association has concluded that Ag/CdO still accounts for 46.7% of the domestic low voltage contactors. So far, relevant base metal ion doped Ag/SnO has not been found 2 Electrical contact materials are present on the market. In order to meet the increasingly strict requirement of 'no cadmium', the provision of Ag/SnO 2 Is an electrical contact material.
For Ag/SnO 2 The wettability between tin oxide and silver is important for the electrical contact performance of the material, and the following three aspects are mainly provided: (1) degree of densification: for powder metallurgy bodies, when wettability between two phases is poor, densification of the material is difficult due to poor phase interface bonding between the second phase of the material and the matrix, while tensile strength of a blank containing 2% porosity is reduced by 50% relative to a blank without porosity; (2) amount of arc ablation: when the electric contact pair is opened and closed, short-time arc discharge can be caused, and under the combined action of local high temperature of an arc, lorentz force and the like, the matrix silver can be melted and splashed to cause quality loss. If the refractory oxide has better wettability with the matrix, the oxide can play a role in stabilizing a silver molten pool and slowing down the splashing of the silver molten pool, thereby reducing the arc ablation amount; (3) contact resistance: during the ablation process, due to the continuous loss of matrix silver, the refractory oxide is gradually enriched on the surface, and in severe cases, local current conduction and disconnection are caused. If the oxide has better wettability with the matrix, the silver molten pool can form good resistance to the enrichment of the oxide, thereby improving the stability of the contact resistance.
Disclosure of Invention
In order to solve the problems, the invention provides a base metal ion doped modified silver tin oxide material which has good two-phase wettability and can reduce the arc ablation amount and improve the contact resistance stability, and a preparation method and application thereof.
The invention provides a base metal ion doped modified silver tin oxide material, which comprises the components of Ag and SnO 2 And an alkali metal, wherein the alkali metal comprises Li, na, and/or K;
the base metal raw material is selected from chloride, nitrate, carbonate, sulfate and acetate of the base metal;
the SnO 2 And the mole percentage of the base metal in the total amount of the base metal is 1-20%; ag. SnO 2 And the total amount of base metals, snO 2 6-15wt.% of alkali metal.
Further, the SnO 2 And the mole percentage of the base metal in the total amount of the base metal is 5-8%; ag. SnO 2 And the total amount of base metals, snO 2 And base metal in total 6-12wt.%.
Further, the SnO 2 And the molar percentage of the base metal in the total amount of the base metal is 5%; ag. SnO 2 And the total amount of base metals, snO 2 And base metal in total 10wt.%.
Further, a self-propagating combustion method or a high-temperature solid-phase sintering method is adopted in the material preparation process;
the invention also provides a preparation method of the base metal ion doped modified silver tin oxide material, which comprises the following steps:
1. preparation of base metal ion doped tin dioxide powder by adopting self-propagating combustion method or high-temperature solid-phase sintering method
(1) Self-propagating combustion process
Dissolving tin chloride, organic fuel and base compound in deionized water, magnetically stirring and mixing for 10-60min, and heating at 300-800 ℃ until self-propagating combustion to obtain base metal ion doped tin dioxide powder;
the base metal in the base compound is selected from lithium, sodium and/or potassium;
(2) Preparing base metal ion doped tin dioxide powder by a high-temperature solid phase sintering method;
uniformly mixing tin dioxide and a basic group compound, drying the powder, and calcining the powder at 500-2000 ℃ for 6-24h to obtain basic group metal ion doped tin dioxide powder;
the base metal in the base compound is selected from lithium, sodium and/or potassium;
2. mixing by a high-energy ball mill to obtain mixed powder
Mixing base metal ion doped tin dioxide powder and silver powder by adopting a high-energy ball mill to obtain mixed powder; in the mixed powder, the content of the base metal ion doped tin dioxide powder is 8-15 wt.%; the ball milling speed of the high-energy ball mill is 100-300 rad/min, the ball milling time is 4h, and the ball-material ratio is (5-10): 1, the mass ratio of the big ball, the middle ball and the small ball is 1:2:2; the diameters of the large ball, the middle ball and the small ball are respectively 10mm, 5mm and 2mm;
3. preliminarily pressing the mixed powder to obtain a blank
The initial pressing is to press the mixed powder into a blank under the pressure of 100-300 MPa, and the pressure maintaining time is not less than 40s;
4. the blank is primarily sintered to obtain a sintered blank
The pre-sintering is to place the blank in a muffle furnace, and sinter the blank for 2 to 4 hours at 860 to 940 ℃ in an air environment to obtain a sintered blank;
5. repressing sintered compact
The repressing pressure is 1000-1200MPa, and the pressure maintaining time is not less than 40s, so that a repressing sintering blank is obtained;
6. re-sintering
And the re-sintering is to place the re-pressed sintering blank in a muffle furnace, and sinter the re-pressed sintering blank for 2 to 4 hours at the temperature of 860 to 940 ℃ in an air environment to obtain the material.
Further, when the self-propagating combustion method is adopted in the first step, the magnetic stirring mixing time is 30min, and the self-propagating combustion temperature is 400-500 ℃.
Further, when the high-temperature solid-phase sintering method is adopted in the first step, the raw materials are calcined at 900-1100 ℃ for 12h.
Further, the base metal salt is selected from chloride, nitrate, carbonate, sulfate and acetate of base metal.
The invention also provides application of the base metal ion doped modified silver tin oxide material in an electric contact material, wherein the material is prepared by adopting the material or the material prepared by the method.
The invention has the beneficial effects that:
the invention discovers that basic metal ions (IA group, L) are predicted through a large amount of experimental research and first-principle calculationi + ，Na + ，K + ) For Ag and SnO 2 The wettability improvement effect is optimal. The electric arc ablation test in a laboratory finds that the alloy is similar to the current Ag/SnO 2 And Ag/SnO 2 /In 2 O 3 In contrast, the base metal ions are doped with Ag/SnO 2 Has lower arc ablation amount, more stable contact resistance and longer electric life. The invention provides base metal ion doped Ag/SnO 2 The electric contact material can be used for assisting in replacing Ag/CdO to be used on a low-voltage apparatus.
Drawings
FIG. 1 shows that metal ions with different bases are doped with SnO 2 An XRD pattern of (a);
FIG. 2 shows that metal ions of different bases are doped with SnO 2 XRD slow scan of (a);
FIG. 3 doping of SnO with different metal ions 2 Wettability with Ag.
Detailed Description
Examples
1. Preparation of base metal ion doped tin dioxide powder by adopting self-propagating combustion method or high-temperature solid-phase sintering method
(1) Self-propagating combustion process
Dissolving tin chloride, organic fuel and basic metal nitrate (such as lithium nitrate, sodium nitrate or potassium nitrate) in deionized water, magnetically stirring and mixing for 30min, and then heating at 400-500 ℃ until self-propagating combustion is carried out to obtain basic metal ion doped tin dioxide powder;
(2) Preparing base metal ion doped tin dioxide powder by a high-temperature solid phase sintering method;
uniformly mixing tin dioxide and basic metal chloride (lithium chloride, sodium chloride or potassium chloride) to obtain basic metal ion doped tin dioxide powder;
2. mixing by a high-energy ball mill to obtain mixed powder
Mixing base metal ion doped tin dioxide powder and silver powder by adopting a high-energy ball mill to obtain mixed powder; in the mixed powder, the content of the base metal ion doped tin dioxide powder is 8-15 wt.%; the ball milling speed of the high-energy ball mill is 100-300 rad/min, the ball milling time is 4h, and the ball material ratio is (5-10): 1, the mass ratio of the big ball, the middle ball and the small ball is 1:2:2; the diameters of the big ball, the middle ball and the small ball are respectively 10mm, 5mm and 2mm;
3. preliminarily pressing the mixed powder to obtain a blank
The initial pressing is to press the mixed powder into a blank under the pressure of 100-300 MPa, and the pressure maintaining time is not less than 40s;
4. the blank is primarily sintered to obtain a sintered blank
The initial sintering is to place the blank in a muffle furnace, and sinter the blank for 2 to 4 hours at 860 to 940 ℃ in an air environment to obtain a sintered blank;
5. repressing sintered compact
The repressing pressure is 1000-1200MPa, and the pressure maintaining time is not less than 40s, so that a repressing sintering blank is obtained;
6. re-sintering
And the re-sintering is to place the re-pressed sintering blank in a muffle furnace, and sinter the re-pressed sintering blank for 2 to 4 hours at the temperature of 860 to 940 ℃ in an air environment to obtain the material.
Comparative example A:
the method comprises the following steps: mixing oxide powder and silver powder by adopting a high-energy ball mill to obtain mixed powder, wherein the oxide powder is Ag/SnO respectively 2 Powder (comparative example 1) and Ag/SnO 2 a/CuO mixed powder (comparative example 2);
in the mixed powder, the content of the oxide powder is 8-15 wt.%;
the process for mixing the base metal ion doped tin dioxide powder and the silver powder by adopting the high-energy ball mill comprises the following steps: the ball milling speed is 100-300 rad/min, the ball milling time is 4h, and the ball material ratio is (5-10): 1, the mass ratio of the big ball, the middle ball and the small ball is 1:2:2; the diameters of the large ball, the middle ball and the small ball are respectively 10mm, 5mm and 2mm;
step two: primarily pressing the mixed powder to obtain a blank;
the initial pressing process comprises the following steps: pressing the mixed powder into a blank under the pressure of 100-300 MPa, and keeping the pressure for not less than 40s;
step three: primarily sintering the blank to obtain a sintered blank;
the primary sintering process comprises the following steps: placing the blank in a muffle furnace, and sintering for 2-4h in air at 860-940 ℃;
step four: re-pressing the sintered blank;
the repressing process comprises the following steps: the pressure is 1000-1200MPa, and the pressure maintaining time is not less than 40s;
step five: re-burning;
the re-sintering process comprises the following steps: and (3) placing the sintering blank obtained by re-pressing in a muffle furnace, and sintering for 2-4h in an air environment at 860-940 ℃.
For examples Ag/SnO 2 :Li，Ag/SnO 2 :Na，Ag/SnO 2 K and comparative Ag/SnO 2 ，Ag/SnO 2 Two contact elements prepared as CuO were subjected to the following comparative tests:
preparation of Ag/SnO 2 The series contact needs to go through four stages of initial pressure, initial burning, re-pressing and re-burning, and Ag/SnO with the same addition amount of oxides 2 For materials, the density of the green compact obtained after initial pressing is generally the same, while the density obtained after initial firing is related to the wettability between the two phases, so that Ag/SnO can be doped by comparing different metal ions 2 Evaluating the wettability of the two phases by the density increment delta d before and after the initial firing of the electric contact material; in addition, for the electrical contact, the compactness of the composite material needs to be more than 95%, otherwise, because the porosity is too high, the strength and the arc ablation resistance of the composite material are greatly reduced, and therefore, the relative density d/d is also tested т (d-Density, d) т Material theoretical density).
The measurement of the two-phase wettability is usually performed by using a high-temperature drop experiment, i.e. the synthesized doped powder is prepared into a large substrate, an Ag block is placed on the substrate, the temperature is raised to be higher than the melting point of Ag under high vacuum, then a high-definition camera is used for recording the spreading condition of Ag on different substrates in the dissolving process, and the trend of wetting angles alpha between different doped oxides and the Ag block is compared, as shown in FIG. 3;
arc ablation test: the test is carried out by using a contact material electrical property simulation system independently developed by Harbin university of industry, and the test conditions are as follows: i =60a, u =380v,
the on-off ratio is 2s:2s. After 6000 ac cycle ablations, the symmetrical contact pair contact resistance R and the electrical contact mass loss G for different materials were compared, and the data listed in table 1 is the average of 5-10 measurements.
As can be seen from Table 1, the base metal ion-doped Ag/SnO prepared in the examples 2 The initial firing density increment of the contact is larger, which reflects that the doping improves the Ag and SnO 2 The wettability of the Ag alloy is that under the action of arc ablation, the oxide has stronger effect of blocking the splashing of the Ag liquid, and the oxide is more difficult to be enriched on the surface, so that the Ag alloy has lower quality loss caused by arc, more stable contact resistance and better electric service life. These all result from the better wettability of the base metal ion doped tin oxide with the matrix. Therefore, compared with the existing method, the reliability and the durability of the contact piece for the low-voltage contactor can be improved.
TABLE 1
FIG. 2 shows that the method successfully prepares high-purity SnO doped with different base metal ions 2 FIG. 3 shows that the doping of low-valence base metal ions can reduce Ag and SnO 2 The wetting angle of the alloy is improved, and the AgSnO is improved 2 Wettability of (3).
Claims (10)
1. A base metal ion doped modified silver tin oxide material is characterized in that: the components of the alloy comprise Ag and SnO 2 And an alkali metal, wherein the alkali metal comprises Li, na, and/or K.
2. The material of claim 1, wherein: the base metal raw material is selected from chloride, nitrate, carbonate, sulfate and acetate of the base metal.
3. The material according to claim 1, wherein the material is selected from the group consisting of,the method is characterized in that: the SnO 2 And the mole percentage of the basic metal is 1-20% in the total amount of the basic metal; ag. SnO 2 And the total amount of alkali metals, snO 2 6-15wt.% of alkali metal.
4. The material of claim 1, wherein: the preparation process of the electric contact material adopts a self-propagating combustion method or a high-temperature solid-phase sintering method.
5. A preparation method of a base metal ion doped modified silver tin oxide material is characterized by comprising the following steps: the method comprises the following steps:
1. preparing base metal ion doped tin dioxide powder by adopting self-propagating combustion method or high-temperature solid-phase sintering method
(1) Self-propagating combustion process
Dissolving tin chloride, organic fuel and base compound in deionized water, magnetically stirring and mixing for 10-60min, and then heating at 300-800 ℃ until self-propagating combustion is achieved to obtain base metal ion doped tin dioxide powder;
the base metal in the base compound is selected from lithium, sodium and/or potassium;
(2) Preparing base metal ion doped tin dioxide powder by a high-temperature solid phase sintering method;
uniformly mixing tin dioxide and a basic group compound, drying the powder, and calcining the powder at 500-2000 ℃ for 6-24h to obtain basic group metal ion doped tin dioxide powder;
the base metal in the base compound is selected from lithium, sodium and/or potassium;
2. mixing by a high-energy ball mill to obtain mixed powder
Mixing base metal ion doped tin dioxide powder and silver powder by adopting a high-energy ball mill to obtain mixed powder; in the mixed powder, the content of the base metal ion doped tin dioxide powder is 8-15 wt.%; the ball milling speed of the high-energy ball mill is 100-300 rad/min, the ball milling time is 4h, and the ball-material ratio is (5-10): 1, the mass ratio of the big ball, the middle ball and the small ball is 1:2:2; the diameters of the large ball, the middle ball and the small ball are respectively 10mm, 5mm and 2mm;
3. preliminarily pressing the mixed powder to obtain a blank
The initial pressing is to press the mixed powder into a blank under the pressure of 100-300 MPa, and the pressure maintaining time is not less than 40s;
4. primarily sintering the blank to obtain a sintered blank
The pre-sintering is to place the blank in a muffle furnace, and sinter the blank for 2 to 4 hours at 860 to 940 ℃ in an air environment to obtain a sintered blank;
5. repressing sintered compact
The repressing pressure is 1000-1200MPa, and the pressure maintaining time is not less than 40s, so that a repressing sintering blank is obtained;
6. re-sintering
And the re-sintering is to place the re-pressed sintering blank in a muffle furnace, and sinter the re-pressed sintering blank for 2 to 4 hours in an air environment at the temperature of 860 to 940 ℃ to obtain the base metal ion doped modified silver tin oxide material.
6. The production method according to claim 5, characterized in that: when the self-propagating combustion method is adopted in the first step, the magnetic stirring and mixing time is 30min, and the self-propagating combustion temperature is 400-500 ℃.
7. The production method according to claim 5, characterized in that: and step one, calcining for 12 hours at 900-1100 ℃ when a high-temperature solid-phase sintering method is adopted.
8. The method of claim 5, wherein: the basic compound is selected from chloride, nitrate, carbonate, sulfate or acetate of basic metal.
9. The method of claim 5, wherein: the alkali metal ion-doped modified silver tin oxide material has the composition as set forth in any one of claims 1 to 4.
10. The application of the basic group metal ion doped modified silver tin oxide material in the electric contact material is characterized in that: the material is as defined in any one of claims 1 to 4 or a material produced by the method as defined in any one of claims 5 to 9.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH116022A (en) * | 1997-06-13 | 1999-01-12 | Sumitomo Metal Mining Co Ltd | Electrical contact material and its production |
| CN101651054A (en) * | 2009-09-11 | 2010-02-17 | 昆明理工大学 | Preparation method of modified AgSnO2 electric contact material |
| CN113957282A (en) * | 2021-10-25 | 2022-01-21 | 哈尔滨工业大学 | Preparation method of metal ion doped modified silver zinc oxide electrical contact material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH116022A (en) * | 1997-06-13 | 1999-01-12 | Sumitomo Metal Mining Co Ltd | Electrical contact material and its production |
| CN101651054A (en) * | 2009-09-11 | 2010-02-17 | 昆明理工大学 | Preparation method of modified AgSnO2 electric contact material |
| CN113957282A (en) * | 2021-10-25 | 2022-01-21 | 哈尔滨工业大学 | Preparation method of metal ion doped modified silver zinc oxide electrical contact material |
Non-Patent Citations (1)
| Title |
|---|
| 马光磊等: "Ag/SnO2 电接触材料的制备及其燃弧特性研究", 《稀有金属材料与工程》 * |
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