CN106312084B - A kind of accuracy control method of tantalum powder also original system - Google Patents

A kind of accuracy control method of tantalum powder also original system Download PDF

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Publication number
CN106312084B
CN106312084B CN201610825430.6A CN201610825430A CN106312084B CN 106312084 B CN106312084 B CN 106312084B CN 201610825430 A CN201610825430 A CN 201610825430A CN 106312084 B CN106312084 B CN 106312084B
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liquid sodium
supply
tantalum powder
plc controller
reduction furnace
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CN106312084A (en
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曾国忠
洪叶荣
梅宏标
月日辉
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Guangdong Guangsheng Photoelectric Rare Metal New Material Co Ltd
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Guangdong Guangsheng Photoelectric Rare Metal New Material Co Ltd
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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
    • 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
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The present invention relates to a kind of accuracy control method of tantalum powder also original system, the tantalum powder also original system further includes a PLC controller, wherein the PLC controller is connected with each other with Liquid Sodium supply container, reduction furnace, Liquid Sodium transfer pump;The control method is controlled using the saturation type of PLC controller, real time reaction raw material flow delivery rate, and automatic speed regulation can be carried out according to pressure in production process, temperature, reach at the uniform velocity effect, it well solves the at the uniform velocity property in tantalum powder reduction process to raw material supply and requires problem, and be fed by the supply of real-time control raw material and segmented, keep reduzate supply in production process accurate, control errors are produced in 100g hereinafter, and being overgauge;The danger coefficient in tantalum powder production process is also reduced simultaneously, reduces manual operation risk, and finally improve product quality, product qualification rate is increased to 99.5% by original 98%.

Description

A kind of accuracy control method of tantalum powder also original system
Technical field:
The present invention relates to tantalum powder technical field of producing, a kind of accuracy control method of tantalum powder also original system is refered in particular to.
Background technology:
Currently, the domestic dosage for carrying out raw material by constant pressure in tantalum powder reduction process is supplied, and by liquid level or Weighing system carries out quantitative calculating, to reach the required amount of production technology.This material quantity Supply Method is primarily present supply The shortcomings of flow velocity is unstable, error is big, manual operation risk is big, while being difficult to the variation according to pressure in production process, temperature The supply of raw material is adjusted, tantalum powder physical property is unstable after causing reduction, or so that production is had danger since raw material supply is excessive It is dangerous.
Invention content:
It is an object of the invention to flow in the prior art, flow velocity are unstable, the deficiencies of making product quality be damaged it Place provides a kind of accuracy control method of tantalum powder also original system.
The technical solution adopted by the present invention is:A kind of accuracy control method of tantalum powder also original system, tantalum powder also original system packet It includes reduction furnace, Liquid Sodium supply container, Liquid Sodium transfer pump and connects their pipeline, reduction furnace is also associated with protection gas supply Pipeline, Liquid Sodium supply container are placed on meausring apparatus, wherein:
The tantalum powder also original system further includes a PLC controller, wherein the title of the PLC controller and Liquid Sodium supply container It is connected with weighing sensor and the first AD converter between amount device;Temperature biography is connected between the PLC controller and reduction furnace Sensor, pressure sensor and the second AD converter;It is connected with D/A converter between the PLC controller and Liquid Sodium transfer pump;
The control method is:
The weight for restoring raw material potassium floutaramite according to tantalum powder first, is obtained by calculation total dosage of required Liquid Sodium, and And reduction furnace temperature, Liquid Sodium flow velocity, flow are set in PLC controller;Reduction furnace prerequisite activity waits for that temperature reaches When setting value, start to supply Liquid Sodium;
When system operation, Liquid Sodium supply container that PLC controller is transmitted according to weighing sensor and the first AD converter Weight difference in 1ms obtains Liquid Sodium actual flow velocity;PLC controller simultaneously according to temperature sensor, pressure sensor and Temperature, pressure data in the reduction furnace of second AD converter transmission find out Liquid Sodium transfer pump using Bernoulli equation calculating Rotating speed, and Liquid Sodium transfer pump is transmitted to by D/A converter, its rotating speed is adjusted, so that liquid sodium flow velocity is reached setting speed Degree, realization are at the uniform velocity supplied;
In the process of running, PLC controller adds up the supply of Liquid Sodium, when its supply reaches the flow of setting, PLC controller control Liquid Sodium transfer pump is out of service, stops feed.
Furthermore, which is added Liquid Sodium using segmented, wherein the first stage:Reduction furnace temperature is set 200 DEG C~220 DEG C fixed, Liquid Sodium supply accounts for the 5%-10% of total amount, and the flow velocity of Liquid Sodium is 4.5kg/min~5.5kg/ min;Second stage, reduction furnace temperature set 590 DEG C~610 DEG C, and Liquid Sodium supply accounts for the 60%~70% of total amount, Liquid Sodium Flow velocity be 3.5kg/min~4.5kg/min;Phase III, reduction furnace temperature set 800 DEG C~820 DEG C, Liquid Sodium supply The 25%~30% of total amount is accounted for, the flow velocity of Liquid Sodium is 3.5kg/min~4.5kg/min;In the above three stage, furnace pressure is restored Power is no more than 3kgf.
Meausring apparatus used in tantalum powder also original system is 3 points of hanging weighing devices in the present invention;Connecting pipe is soft Pipe;Liquid Sodium transfer pump uses electromagnetic pump.Weighting error can be reduced using hose connection.
Control method of the present invention is controlled using the saturation type of PLC controller, real time reaction raw material flow delivery rate, and Automatic speed regulation can be carried out according to pressure in production process, temperature, reach at the uniform velocity effect, well solve tantalum powder reduction process In problem is required to the at the uniform velocity property of raw material supply, and be fed by the supply of real-time control raw material and segmented, make production Reduzate supply is accurate in the process, and production control errors are in 100g hereinafter, and being overgauge;Tantalum powder is also reduced simultaneously to produce Danger coefficient in journey reduces manual operation risk, and finally improves product quality, and product qualification rate is carried by original 98% Height is to 99.5%.
Description of the drawings:
Fig. 1 is the flow chart of control method of the present invention;
Fig. 2 is the composition schematic diagram of tantalum powder also original system in the present invention.
Specific implementation mode:
With reference to specific embodiments and the drawings, the present invention is further described.
In conjunction with shown in Fig. 1~Fig. 2, the accuracy control method of a kind of tantalum powder also original system in the present embodiment, tantalum powder reduction system System includes reduction furnace, Liquid Sodium supply container, Liquid Sodium transfer pump and connects their pipeline, and reduction furnace is also associated with protection gas Supply line, Liquid Sodium supply container are placed on meausring apparatus, wherein:
The tantalum powder also original system further includes a PLC controller, wherein the title of the PLC controller and Liquid Sodium supply container It is connected with weighing sensor and the first AD converter between amount device;Temperature biography is connected between the PLC controller and reduction furnace Sensor, pressure sensor and the second AD converter;It is connected with D/A converter between the PLC controller and Liquid Sodium transfer pump;
The control method is:
The weight for restoring raw material potassium floutaramite according to tantalum powder first, is obtained by calculation total dosage of required Liquid Sodium, and And reduction furnace temperature, Liquid Sodium flow velocity, flow are set in PLC controller;Reduction furnace prerequisite activity waits for that temperature reaches When setting value, start to supply Liquid Sodium;
When system operation, Liquid Sodium supply container that PLC controller is transmitted according to weighing sensor and the first AD converter Weight difference in 1ms obtains Liquid Sodium actual flow velocity;PLC controller simultaneously according to temperature sensor, pressure sensor and Temperature, pressure data in the reduction furnace of second AD converter transmission find out Liquid Sodium transfer pump using Bernoulli equation calculating Rotating speed, and Liquid Sodium transfer pump is transmitted to by D/A converter, its rotating speed is adjusted, so that liquid sodium flow velocity is reached setting speed Degree, realization are at the uniform velocity supplied;
In the process of running, PLC controller adds up the supply of Liquid Sodium, when its supply reaches the flow of setting, PLC controller control Liquid Sodium transfer pump is out of service, stops feed.
Furthermore, which is added Liquid Sodium using segmented, wherein the first stage:Reduction furnace temperature is set 200 DEG C~220 DEG C fixed, Liquid Sodium supply accounts for the 5%-10% of total amount, and the flow velocity of Liquid Sodium is 4.5kg/min~5.5kg/ min;Second stage, reduction furnace temperature set 590 DEG C~610 DEG C, and Liquid Sodium supply accounts for the 60%~70% of total amount, Liquid Sodium Flow velocity be 3.5kg/min~4.5kg/min;Phase III, reduction furnace temperature set 800 DEG C~820 DEG C, Liquid Sodium supply The 25%~30% of total amount is accounted for, the flow velocity of Liquid Sodium is 3.5kg/min~4.5kg/min;In the above three stage, furnace pressure is restored Power is no more than 3kgf.
Meausring apparatus used in tantalum powder of the present invention also original system is 3 points of hanging weighing devices;Connecting pipe is soft Pipe;Liquid Sodium transfer pump uses electromagnetic pump.Weighting error can be reduced using hose connection.
Application Example:
Restore 50kg potassium floutaramites, in three times plus reducing agent Liquid Sodium, reduction furnace temperature is respectively 210 DEG C, 600 DEG C, 810 DEG C, addition is respectively 2kg, 20kg, 8kg, Liquid Sodium flow velocity be respectively 5kg/min at the uniform velocity, 4kg/min at the uniform velocity, 4kg/min it is even Speed;Pressure is no more than 3kgf in reduction furnace;Using control method of the present invention, in implementation process, rate change rate is no more than 10%, weight error is strict controlled in 100g hereinafter, and being overgauge.
Control method of the present invention is controlled using the saturation type of PLC controller, real time reaction raw material flow delivery rate, and Automatic speed regulation can be carried out according to pressure in production process, temperature, reach at the uniform velocity effect, well solve tantalum powder reduction process In problem is required to the at the uniform velocity property of raw material supply, and be fed by the supply of real-time control raw material and segmented, make production Reduzate supply is accurate in the process, and production control errors are in 100g hereinafter, and being overgauge;Tantalum powder is also reduced simultaneously to produce Danger coefficient in journey reduces manual operation risk, and finally improves product quality, and product qualification rate is carried by original 98% Height is to 99.5%.

Claims (2)

1. a kind of accuracy control method of tantalum powder also original system, tantalum powder also original system includes reduction furnace, Liquid Sodium supply container, liquid State sodium transfer pump and the pipeline for connecting them, reduction furnace are also associated with protection gas supply line, and Liquid Sodium supply container is placed in title It measures on device, it is characterised in that:
The tantalum powder also original system further includes a PLC controller, wherein the PLC controller and the weighing of Liquid Sodium supply container fill Weighing sensor and the first AD converter are connected between setting;Be connected between the PLC controller and reduction furnace temperature sensor, Pressure sensor and the second AD converter;It is connected with D/A converter between the PLC controller and Liquid Sodium transfer pump;
The control method is:
The weight for restoring raw material potassium floutaramite according to tantalum powder first, is obtained by calculation total dosage of required Liquid Sodium, and Reduction furnace temperature, Liquid Sodium flow velocity, flow are set in PLC controller;Reduction furnace prerequisite activity waits for that temperature reaches setting When value, start to supply Liquid Sodium;
When system operation, the Liquid Sodium supply container that PLC controller is transmitted according to weighing sensor and the first AD converter is in 1ms Interior weight difference obtains Liquid Sodium actual flow velocity;PLC controller is simultaneously according to temperature sensor, pressure sensor and second Temperature, pressure data in the reduction furnace of AD converter transmission find out Liquid Sodium using Bernoulli equation calculating and supply revolution speed, And Liquid Sodium transfer pump is transmitted to by D/A converter, its rotating speed is adjusted, so that liquid sodium flow velocity is reached setting speed, it is real Now at the uniform velocity supply;
In the process of running, PLC controller adds up the supply of Liquid Sodium, when its supply reaches the flow of setting, PLC controls Device control Liquid Sodium transfer pump processed is out of service, stops feed;
Liquid Sodium is added using segmented in the control method, wherein the first stage:It restores furnace temperature and sets 200 DEG C ~ 220 DEG C, liquid State sodium supply accounts for the 5%-10% of total amount, and the flow velocity of Liquid Sodium is 4.5kg/min ~ 5.5kg/min;Second stage restores furnace temperature 590 DEG C ~ 610 DEG C of degree setting, Liquid Sodium supply account for the 60% ~ 70% of total amount, and the flow velocity of Liquid Sodium is 3.5kg/min ~ 4.5kg/ min;Phase III, reduction furnace temperature set 800 DEG C ~ 820 DEG C, and Liquid Sodium supply accounts for the 25% ~ 30% of total amount, the stream of Liquid Sodium Speed is 3.5kg/min ~ 4.5kg/min;In the above three stage, reduction furnace pressure is no more than 3kgf.
2. the accuracy control method of tantalum powder according to claim 1 also original system, it is characterised in that:In tantalum powder also original system Meausring apparatus used is 3 points of hanging weighing devices;Connecting pipe is hose;Liquid Sodium transfer pump uses electromagnetic pump.
CN201610825430.6A 2016-09-14 2016-09-14 A kind of accuracy control method of tantalum powder also original system Active CN106312084B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101574741A (en) * 2009-06-25 2009-11-11 宁夏东方钽业股份有限公司 Preparation method of tantalum powder for capacitor
CN102990076A (en) * 2012-12-18 2013-03-27 宁夏东方钽业股份有限公司 Stirring water-washing method and device for producing tantalum powder by reducing potassium fluotantalate via metallic sodium
CN204700313U (en) * 2015-05-18 2015-10-14 江门富祥电子材料有限公司 A kind of device of sodium reduction potassium floutaramite
CN204924333U (en) * 2015-09-11 2015-12-30 株洲硬质合金集团有限公司 Liquid sodium metering device

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3871824B2 (en) * 1999-02-03 2007-01-24 キャボットスーパーメタル株式会社 Tantalum powder for high capacity capacitors

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101574741A (en) * 2009-06-25 2009-11-11 宁夏东方钽业股份有限公司 Preparation method of tantalum powder for capacitor
CN102990076A (en) * 2012-12-18 2013-03-27 宁夏东方钽业股份有限公司 Stirring water-washing method and device for producing tantalum powder by reducing potassium fluotantalate via metallic sodium
CN204700313U (en) * 2015-05-18 2015-10-14 江门富祥电子材料有限公司 A kind of device of sodium reduction potassium floutaramite
CN204924333U (en) * 2015-09-11 2015-12-30 株洲硬质合金集团有限公司 Liquid sodium metering device

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