CN110527863A - A kind of preparation method of silver titanium contact material - Google Patents

A kind of preparation method of silver titanium contact material Download PDF

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Publication number
CN110527863A
CN110527863A CN201910807516.XA CN201910807516A CN110527863A CN 110527863 A CN110527863 A CN 110527863A CN 201910807516 A CN201910807516 A CN 201910807516A CN 110527863 A CN110527863 A CN 110527863A
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Prior art keywords
silver
contact material
colored titanium
titanium
colored
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Inventor
刘松涛
王俊勃
贺辛亥
侯海云
杨敏鸽
付翀
思芳
杨凯
师浩军
周辛梓
蔺鑫璐
游义博
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Xian Polytechnic University
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Xian Polytechnic University
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Priority to CN201910807516.XA priority Critical patent/CN110527863A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0466Alloys based on noble metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/06Alloys based on silver

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Contacts (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a kind of preparation method of silver-colored titanium contact material, specifically: firstly, choosing the titanium valve that granularity is 100~500 mesh;Silver ammino solution is prepared using silver nitrate solution and ammonium hydroxide;Titanium valve addition silver ammino solution is uniformly mixed again, and prepares silver-colored titanium composite granule in conjunction with chemical deposition using reducing agent;Finally silver-colored titanium composite granule is successively formed, sintering processes, silver-colored titanium contact material can be obtained.The silver-colored titanium contact material being evenly distributed is made using chemical deposition by the present invention, and the dosage of silver is controlled in 60%~90% range, and the dosage of silver can be effectively reduced, reduce costs.

Description

A kind of preparation method of silver titanium contact material
Technical field
The invention belongs to technical field of composite preparation, and in particular to a kind of preparation method of silver titanium contact material.
Background technique
Contact material plays irreplaceable role in complicated circuit system, and service performance transports the safety of circuit Row has decisive influence.And silver-based electric contact material is because its good service performance is widely used in low-voltage electrical apparatus, in electricity Vital effect is played in the use of device.Currently, common silver-based electric contact material mainly has silver metal to be in electrical contact material Material and silver oxide (Ag/MeO) contact material, such as Ag/Ni, Ag/SnO2, Ag/CuO etc., these silver-based electric contact materials Relatively good effect has been played in use.But the use content that existing silver-based electric contact material has silver is high This problem, leads to the higher cost of final products, and preparation process requires the disadvantages of stringenter, makes the industrialization of contact material Application cost is higher.
Summary of the invention
The purpose of the present invention is to provide a kind of silver-colored titanium contact material preparation methods, solve existing contact material and exist Poor in processability and the higher problem of silver content in preparation process.
The technical scheme adopted by the invention is that a kind of preparation method of silver titanium contact material, specifically according to following step It is rapid to implement:
Step 1 chooses the titanium valve that granularity is 100~500 mesh;
Step 2 prepares silver ammino solution using silver nitrate solution and ammonium hydroxide;
Silver ammino solution prepared by the titanium valve addition step 2 in step 1 is uniformly mixed, and utilizes reducing agent by step 3, knot Chemical deposition is closed, silver-colored titanium composite granule is prepared;
Step 4, the silver-colored titanium composite granule for obtaining step 3 successively formed, sintering processes, and silver-colored titanium electricity can be obtained and connect Touch material.
The features of the present invention also characterized in that
In step 2, it is specifically implemented according to the following steps:
The silver nitrate that mass ratio is 1~5:95~99 is uniformly mixed by step 2.1 with water, and it is molten to obtain clear silver nitrate Liquid;
Ammonium hydroxide is slowly dropped in the silver nitrate solution obtained after step 2.1 by step 2.2, forms silver ammino solution, and During dropwise addition, the pH value of solution is controlled between 7~11.
In step 3, it is specifically implemented according to the following steps:
Step 3.1 presses titanium elements and silver element molar ratio as 1:1.09~8.4, and the titanium valve in step 1 is added to step In the silver ammino solution formed in 2, after mixing evenly, finely dispersed suspension system is obtained;
Reducing agent is slowly dropped in the suspension system obtained through step 3.1 by step 3.2, is stirred using when being added dropwise Mode, during dropwise addition using hydrochloric acid examine suspension in silver ion, until suspension in without silver ion exist, stop drop Add reducing agent, silver-colored titanium composite granule is prepared.
Reducing agent is hydrazine hydrate, ascorbic acid, glucose, formaldehyde, acetaldehyde, glyoxal, formic acid, formates, formic acid rouge, second Any one in acid, boron hydracid sodium, sodium dithionite.
In step 4, specifically: the silver-colored titanium composite granule obtained through step 3 is pressed into working process through hot extrusion technique or again, Vacuum annealing process 1h~3h at a temperature of 500 DEG C~700 DEG C later, can be obtained silver-colored titanium contact material.
The beneficial effects of the present invention are:
1. chemical deposition involved in silver-colored titanium contact material preparation method of the invention, can be most using chemical deposition The agglomeration of titanium valve is reduced in limits;
2. the silver-colored titanium contact material of the method for the present invention preparation, improves the processability of contact material;
3. the silver-colored titanium contact material that is evenly distributed is made using chemical deposition, by the dosage control of silver 60%~ In 90% range, the dosage of silver can be effectively reduced, reduce costs.
Specific embodiment
The present invention is described in detail With reference to embodiment.
A kind of preparation method of silver-colored titanium contact material of the present invention, is specifically implemented according to the following steps:
Step 1 chooses the titanium valve that granularity is 100~500 mesh;
Step 2 prepares silver ammino solution using silver nitrate solution and ammonium hydroxide, is specifically implemented according to the following steps:
The silver nitrate that mass ratio is 1~5:95~99 is uniformly mixed by step 2.1 with water, and it is molten to obtain clear silver nitrate Liquid;
Ammonium hydroxide is slowly dropped in the silver nitrate solution obtained after step 2.1 by step 2.2, forms silver ammino solution, and During dropwise addition, the pH value of solution is controlled between 7~11;
Silver ammino solution prepared by the titanium valve addition step 2 in step 1 is uniformly mixed, and utilizes reducing agent by step 3, knot Chemical deposition is closed, silver-colored titanium composite granule is prepared, is specifically implemented according to the following steps:
Step 3.1 presses titanium elements and silver element molar ratio as 1:1.09~8.4, and the titanium valve in step 1 is added to step In the silver ammino solution formed in 2, after mixing evenly, finely dispersed suspension system is obtained;
Agitating mode is that mechanical stirring, airflow stirring or mechanical stirring add ultrasonic disperse;
Reducing agent is slowly dropped in the suspension system obtained through step 3.1 by step 3.2, is stirred using when being added dropwise Mode, during dropwise addition using hydrochloric acid examine suspension in silver ion, until suspension in without silver ion exist, stop drop Add reducing agent, silver-colored titanium composite granule is prepared;
Wherein, reducing agent is hydrazine hydrate, ascorbic acid, glucose, formaldehyde, acetaldehyde, glyoxal, formic acid, formates, formic acid Rouge, acetic acid, boron hydracid sodium, any one in sodium dithionite;
Step 4, the silver-colored titanium composite granule for obtaining step 3 successively formed, sintering processes, obtains silver-colored titanium electrical contact material Material, specifically:
The silver-colored titanium composite granule obtained through step 3 is pressed into working process through hot extrusion technique or again, later in 500 DEG C~ Silver-colored titanium contact material can be obtained to adjust finished product hardness in vacuum annealing process 1h~3h at a temperature of 700 DEG C.
Embodiment 1
A kind of preparation method of silver-colored titanium contact material of the present invention, is specifically implemented according to the following steps:
Step 1 chooses the titanium valve that partial size is 150 mesh;
Step 2 is that 1:99 weighs silver nitrate and water respectively, and weighed silver nitrate is uniformly mixed with water in mass ratio, Obtain clear silver nitrate solution;And ammonium hydroxide is slowly dropped in silver nitrate solution, silver ammino solution is formed, in the process of dropwise addition In, using the pH value of pH meter control solution 7.5;
Step 3 presses titanium elements and silver element molar ratio as 1:3.5, and titanium valve is added in silver ammino solution, is stirred evenly Afterwards, finely dispersed suspension system is obtained;
Reducing agent-hydrazine hydrate is slowly dropped in suspension system, by the way of being stirred when being added dropwise, in the process of dropwise addition It is middle to examine silver ion in suspension using hydrochloric acid, until existing in suspension without silver ion, stop that reducing agent-hydrazine hydrate is added dropwise, Silver-colored titanium composite granule is prepared;
Silver-colored titanium composite granule is pressed working process through hot extrusion technique or again by step 4, obtains receiving silver-colored titanium contact material; By silver-colored titanium contact material at a temperature of 500 DEG C vacuum annealing process 3h, connect to adjust finished product hardness to get to silver-colored titanium electricity Touch material.
Embodiment 2
A kind of preparation method of silver-colored titanium contact material of the present invention, is specifically implemented according to the following steps:
Step 1 chooses the titanium valve that partial size is 180 mesh;
Step 2 is that 2:98 weighs silver nitrate and water respectively, and weighed silver nitrate is uniformly mixed with water in mass ratio, Obtain clear silver nitrate solution;Ammonium hydroxide is taken, and ammonium hydroxide is slowly dropped in silver nitrate solution, silver ammino solution is formed, is dripping During adding, using the pH value of pH meter control solution 8;
Step 3 presses titanium elements and silver element molar ratio as 1:6, and titanium valve is added in silver ammino solution, after mixing evenly, Obtain finely dispersed suspension system;
Reducing agent-ascorbic acid is slowly dropped in suspension system, by the way of being stirred when being added dropwise, had been added dropwise Silver ion in suspension is examined using hydrochloric acid in journey, until existing in suspension without silver ion, stops that reducing agent-Vitamin C is added dropwise Silver-colored titanium composite granule is prepared in acid;
Silver-colored titanium composite granule is pressed working process through hot extrusion technique or again by step 4, obtains silver-colored titanium contact material;It will Silver-colored titanium contact material vacuum annealing process 2h at a temperature of 600 DEG C is in electrical contact to adjust finished product hardness to get to silver-colored titanium Material.
Embodiment 3
A kind of preparation method of silver-colored titanium contact material of the present invention, is specifically implemented according to the following steps:
Step 1 chooses the titanium valve that partial size is 200 mesh;
Step 2 is that 3:97 weighs silver nitrate and water respectively, and weighed silver nitrate is uniformly mixed with water in mass ratio, Obtain clear silver nitrate solution;Ammonium hydroxide is taken, and ammonium hydroxide is slowly dropped in silver nitrate solution, silver ammino solution is formed, is dripping During adding, using the pH value of pH meter control solution 8.2;
Step 3 presses titanium elements and silver element molar ratio as 1:6, and titanium valve is added in silver ammino solution, after mixing evenly, Obtain finely dispersed suspension system;
Reducing agent-formaldehyde is slowly dropped in suspension system, by the way of being stirred when being added dropwise, during dropwise addition Silver ion in suspension is examined using hydrochloric acid, until existing in suspension without silver ion, stops that reducing agent-formaldehyde, preparation is added dropwise Obtain silver-colored titanium composite granule;
Silver-colored titanium composite granule is pressed working process through hot extrusion technique or again by step 4, obtains silver-colored titanium contact material;It will Silver-colored titanium contact material vacuum annealing process 1h at a temperature of 700 DEG C is in electrical contact to adjust finished product hardness to get to silver-colored titanium Material.
Embodiment 4
A kind of preparation method of silver-colored titanium contact material of the present invention, is specifically implemented according to the following steps:
Step 1 chooses the titanium valve that partial size is 250 mesh;
Step 2 is that 4:95 weighs silver nitrate and water respectively, and weighed silver nitrate is uniformly mixed with water in mass ratio, Obtain clear silver nitrate solution;Ammonium hydroxide is taken, and ammonium hydroxide is slowly dropped in silver nitrate solution, silver ammino solution is formed, is dripping During adding, using the pH value of pH meter control solution 11;
Step 3 presses titanium elements and silver element molar ratio as 1:9, and titanium valve is added in silver ammino solution, after mixing evenly, Obtain finely dispersed suspension system;
Reducing agent-acetaldehyde is slowly dropped in suspension system, by the way of being stirred when being added dropwise, during dropwise addition Silver ion in suspension is examined using hydrochloric acid, until existing in suspension without silver ion, stops that reducing agent-acetaldehyde, preparation is added dropwise Obtain silver-colored titanium composite granule;
Silver-colored titanium composite granule is pressed working process through hot extrusion technique or again by step 4, obtains silver-colored titanium contact material;It will Silver-colored titanium contact material vacuum annealing process 1.5h at a temperature of 650 DEG C connects to adjust finished product hardness to get to silver-colored titanium electricity Touch material.
Embodiment 5
A kind of preparation method of silver-colored titanium contact material of the present invention, is specifically implemented according to the following steps:
Step 1 chooses the titanium valve that partial size is 350 mesh;
Step 2 is that 5:96 weighs silver nitrate and water respectively, and weighed silver nitrate is uniformly mixed with water in mass ratio, Obtain clear silver nitrate solution;Ammonium hydroxide is taken, and ammonium hydroxide is slowly dropped in silver nitrate solution, silver ammino solution is formed, is dripping During adding, using the pH value of pH meter control solution 10;
Step 3 presses titanium elements and silver element molar ratio as 1:12, and titanium valve is added in silver ammino solution, after mixing evenly, Obtain finely dispersed suspension system;
Reducing agent-formates is slowly dropped in suspension system, by the way of being stirred when being added dropwise, in the process of dropwise addition It is middle to examine silver ion in suspension using hydrochloric acid, until existing in suspension without silver ion, stop that reducing agent-formates is added dropwise, Silver-colored titanium composite granule is prepared;
Silver-colored titanium composite granule is pressed working process through hot extrusion technique or again by step 4, obtains silver-colored titanium contact material;It will Silver-colored titanium contact material vacuum annealing process 2.5h at a temperature of 550 DEG C connects to adjust finished product hardness to get to silver-colored titanium electricity Touch material.
Embodiment 6
A kind of preparation method of silver-colored titanium contact material of the present invention, is specifically implemented according to the following steps:
Step 1 chooses the titanium valve that partial size is 300 mesh;
Step 2 is that 5:99 weighs silver nitrate and water respectively, and weighed silver nitrate is uniformly mixed with water in mass ratio, Obtain clear silver nitrate solution;Ammonium hydroxide is taken, and ammonium hydroxide is slowly dropped in silver nitrate solution, silver ammino solution is formed, is dripping During adding, using the pH value of pH meter control solution 9;
Step 3 is that titanium valve is added in silver ammino solution by 1:12.5 by titanium elements and silver element molar ratio, is stirred evenly Afterwards, finely dispersed suspension system is obtained;
Reducing agent-boron hydracid sodium salt is slowly dropped in suspension system, by the way of being stirred when being added dropwise, is being added dropwise Silver ion in suspension is examined using hydrochloric acid in the process, until existing in suspension without silver ion, stops that reducing agent-boron hydrogen is added dropwise Silver-colored titanium composite granule is prepared in sour sodium;
Silver-colored titanium composite granule is pressed working process through hot extrusion technique or again by step 4, obtains silver-colored titanium contact material;It will Silver-colored titanium contact material vacuum annealing process 1.5h at a temperature of 700 DEG C connects to adjust finished product hardness to get to silver-colored titanium electricity Touch material.
The lightweight silver titanium electricity being evenly distributed is made silver-colored titanium contact material preparation method of the invention using chemical deposition The dosage of silver can be effectively reduced in contact material;In addition, solving existing contact material, existing titanium valve is inclined during the preparation process The problem of poly- and poor in processability.When the Ag/Ti contact material of silver content 80% is made using chemical deposition process, detect Density is 7.4g/cm, and hardness can reach 134.3HV, and conductivity is in 30.0%IACS or more, and Tissue distribution is uniform.

Claims (5)

1. a kind of preparation method of silver titanium contact material, which is characterized in that be specifically implemented according to the following steps:
Step 1 chooses the titanium valve that granularity is 100~500 mesh;
Step 2 prepares silver ammino solution using silver nitrate solution and ammonium hydroxide;
Silver ammino solution prepared by the titanium valve addition step 2 in step 1 is uniformly mixed, and utilizes reducing agent by step 3, in conjunction with change Sedimentation is learned, silver-colored titanium composite granule is prepared;
Step 4, the silver-colored titanium composite granule for obtaining step 3 successively formed, sintering processes, and silver-colored titanium electrical contact material can be obtained Material.
2. a kind of preparation method of silver-colored titanium contact material according to claim 1, which is characterized in that in the step 2, It is specifically implemented according to the following steps:
The silver nitrate that mass ratio is 1~5:95~99 is uniformly mixed by step 2.1 with water, obtains clear silver nitrate solution;
Ammonium hydroxide is slowly dropped in the silver nitrate solution obtained after step 2.1 by step 2.2, forms silver ammino solution, and dripping During adding, the pH value of solution is controlled between 7~11.
3. a kind of preparation method of silver-colored titanium contact material according to claim 1, which is characterized in that in the step 3, It is specifically implemented according to the following steps:
Step 3.1 presses titanium elements and silver element molar ratio as 1:1.09~8.4, and the titanium valve in step 1 is added in step 2 In the silver ammino solution of formation, after mixing evenly, finely dispersed suspension system is obtained;
Reducing agent is slowly dropped in the suspension system obtained through step 3.1 by step 3.2, using the side stirred when being added dropwise Formula examines silver ion in suspension using hydrochloric acid during dropwise addition, until existing in suspension without silver ion, stops being added dropwise also Silver-colored titanium composite granule is prepared in former agent.
4. a kind of preparation method of silver-colored titanium contact material according to claim 3, which is characterized in that the reducing agent is Hydrazine hydrate, glucose, formaldehyde, acetaldehyde, glyoxal, formic acid, formates, formic acid rouge, acetic acid, boron hydracid sodium, connects two at ascorbic acid Any one in sodium sulfite.
5. a kind of preparation method of silver-colored titanium contact material according to claim 1, which is characterized in that in the step 4, Specifically: the silver-colored titanium composite granule obtained through step 3 is pressed into working process through hot extrusion technique or again, later in 500 DEG C~700 Silver-colored titanium contact material can be obtained in vacuum annealing process 1h~3h at a temperature of DEG C.
CN201910807516.XA 2019-08-29 2019-08-29 A kind of preparation method of silver titanium contact material Pending CN110527863A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1278015A (en) * 1999-06-22 2000-12-27 章景兴 Electric contact material alloy based on silver-titanium and prodn. process therefor
CN1558432A (en) * 2004-02-12 2004-12-29 章景兴 Ag-Ni-Ti based electrical contact material and its manufacturing process
CN106191495A (en) * 2016-07-12 2016-12-07 西安工程大学 The tin-oxygen-silver electric contact material preparation method of chemically based sedimentation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1278015A (en) * 1999-06-22 2000-12-27 章景兴 Electric contact material alloy based on silver-titanium and prodn. process therefor
CN1558432A (en) * 2004-02-12 2004-12-29 章景兴 Ag-Ni-Ti based electrical contact material and its manufacturing process
CN106191495A (en) * 2016-07-12 2016-12-07 西安工程大学 The tin-oxygen-silver electric contact material preparation method of chemically based sedimentation

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Application publication date: 20191203