CN101782497A - Device for high-temperature sulfidation attack experiment of material - Google Patents

Device for high-temperature sulfidation attack experiment of material Download PDF

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Publication number
CN101782497A
CN101782497A CN 201010121392 CN201010121392A CN101782497A CN 101782497 A CN101782497 A CN 101782497A CN 201010121392 CN201010121392 CN 201010121392 CN 201010121392 A CN201010121392 A CN 201010121392A CN 101782497 A CN101782497 A CN 101782497A
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China
Prior art keywords
container
experimental provision
temperature
material according
sulfidation attack
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CN 201010121392
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Chinese (zh)
Inventor
刘志坚
王辉
黄海锋
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Central South University
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Central South University
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Priority to CN 201010121392 priority Critical patent/CN101782497A/en
Publication of CN101782497A publication Critical patent/CN101782497A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a device for the high-temperature sulfidation attack experiment of materials. A support is arranged in a container with a cover plate (2). Fine wire hooks used for hanging samples are arranged on the support. A certain amount of elemental sulfur (9) is placed at the bottom end of the container. The container is connected with a vacuum system and an argon inflation system. A heating system is arranged in a heating way corresponding to the fine wire hooks arranged in the container and used for hanging samples. One another heating system is arranged in a heating way corresponding to the elemental sulfur (9) placed at the bottom end of the container. The invention has the advantages that the structure is simple, the manufacturing cost is low, the operation is simple, the experiment can be conducted to a plurality of samples, the sulfur pressure can be freely controlled and the device is suitable for sulfidation experiments in the elemental sulfur atmosphere below 1000 DEG C.

Description

The high-temperature sulfidation attack experimental provision that is used for material
Technical field
The present invention relates to a kind of device that the decay resistance of material is tested of being used for, be specifically related to a kind of high-temperature sulfidation attack experimental provision that is used for material.
Background technology
The high temperature vulcanized of metal material generally occurs in the equipment that uses mineral fuel and energy conversion, relates to modern industries such as aviation, petrochemical complex, thermal power generation, coal gasification.The high temperature vulcanized speed of metal is than fast many of its oxidation rate, and harmfulness is very big.
In order to study the high temperature vulcanized mechanism of metal, need in specific sulfuration experimental provision, measure the corrosion kinetics under high temperature sulphur atmosphere of metal.The high temperature sulphur environment of realizing in the experimental provision generally has two kinds, and a kind of is the volatilization of solid elemental sulfur, and it is 1~10 that may command sulphur is pressed -2Atm, another kind adopt H 2S-H 2Atmosphere, may command sulphur is pressed wider range, is about 10 -2~10 -10Atm.H 2S-H 2The sulphur pressure ratio that atmosphere realizes is less, and the equipment that experiment needs is more, complicated operation; The attainable sulphur of the volatilization of solid sulfur is pressed higher, but then solidifies owing to the elemental sulfur chance is cold, and being easy to influences experimental result attached on the experimental provision.
Mostly be to adopt the volatilization of elemental sulfur to come designing apparatus both at home and abroad, its core component is exactly the quartz spring thermobalance.The characteristics of this equipment are exactly can the weightening finish of continuous coverage sample in corrosion process, and absolute precision is higher.But the equipment complexity, cost of manufacture is higher, and once can only measure a sample, can not realize the contrast of a plurality of samples under same environment, and especially relatively more responsive to vulcanization environment simple metal is as pure nickel etc.
Summary of the invention
Technical matters to be solved by this invention provides a kind of easy, and cost of manufacture is low, and is practical, the high-temperature sulfidation attack experimental provision that is used for material that can experimentize to a plurality of samples simultaneously.
In order to solve the problems of the technologies described above, the present invention is a kind of high-temperature sulfidation attack experimental provision that is used for material, have in the container of cover plate and be provided with support, described support is provided with the filament hook that is used to hang sample, the bottom of described container is placed with the simple substance sulphur of certain mass, described container is connected with one group of vacuum system and one group of argon gas gas charging system, one group of heating system is provided with the corresponding heating of filament hook that sample is hung in interior being used to of described container, and another group heating system is provided with the corresponding heating of simple substance sulphur that place the bottom of described container.
The top of described support is provided with thermofin.
Every group of described heating system is made of a temperature controller, a thermopair and a resistance furnace respectively, and described temperature controller connects a described thermopair, the described resistance furnace of the corresponding measurement of described thermopair.
Described container is a rustless steel container.Described support is a stainless steel stent.Described filament hook is the stainless steel filament hook.Described thermofin is the stainless steel thermofin.
Described argon gas gas charging system is made up of argon bottle and the bumping bag on the export pipeline that is located at described argon bottle.
Adopt the high-temperature sulfidation attack experimental provision that is used for material of technique scheme, have cover plate rustless steel container, two groups of resistance furnaces, thermopair and temperature controllers, have the vacuum system of argon bottle, in rustless steel container outside, one group of resistance furnace and thermopair are positioned at the place of stainless steel filament hook hook; Another group is positioned at container bottom.Every group of described heating system is made of temperature controller, thermopair and a resistance furnace respectively, one group is used to control the sulfidation corrosion temperature, one group of heating system is being controlled the temperature of sulphur, utilizes the saturated vapor pressure of sulphur and the relation of temperature to control the interior sulphur pressure of rustless steel container; Vacuum system comprises vacuum pump, pipeline, valve, is used for removing oxygen and nitrogen with the rustless steel container the inside before the corrosion.Argon bottle and bumping bag guarantee that the atmosphere in the preceding rustless steel container of corrosion is an about atmospheric argon gas.Be placed with thermofin on the support in the rustless steel container, be used for guaranteeing that corrosion temperature is constant on the one hand, be used for hanging sample on the other hand and stop that sulphur steam permeates upward.
In order to guarantee the sealing of container, the leather washer that scribbles vacuum grease is arranged between cover plate and container.
The present invention is specially at the high temperature vulcanized dynamic (dynamical) experimental provision of non-continuous, can realize same temperature, and it is high temperature vulcanized that different sulphur are depressed, and can realize that also same sulphur presses, high temperature vulcanized under the different temperatures.Can regulate being no more than 1000 ℃ corrosion temperature, control sulphur by the temperature of regulating simple substance sulphur and press, controlled sulphur pressure scope is 1~10 -2Atm.
The present invention is simple in structure, and is with low cost, easy to operate, can carry out under same corrosion environment a plurality of samples simultaneously high temperature vulcanized, the comparative height of experiment.After stopping heating,, can realize that sulphur steam solidifies recovery in the bottom, prevent it, improve the precision of experiment attached to sample surfaces by to rustless steel container bottom water-cooled.
Description of drawings
Fig. 1 is an experimental provision structural representation of the present invention.
Embodiment
Below in conjunction with accompanying drawing in detail the present invention is described in detail.
With reference to Fig. 1, have in the rustless steel container 1 of cover plate 2 and be provided with stainless steel stent 10, be placed with stainless steel thermofin 11 at the top of stainless steel stent 10, be on the stainless steel stent 10 stainless steel thermofin 11 below be provided with the stainless steel filament hook 17 that is used to hang sample, the bottom of rustless steel container 1 is placed with the simple substance sulphur 9 of certain mass, in order to guarantee the sealing of container, at cover plate 2 and 1 of rustless steel container the leather washer that scribbles vacuum grease is arranged, rustless steel container 1 links to each other with vacuum pump 12 with argon bottle 15 by rubber tubing 16, the export pipeline of argon bottle 15 is provided with bumping bag 14, and the outlet of vacuum pump 12 is provided with valve 13; First resistance furnace 3 is provided with the stainless steel filament hook 17 corresponding heating that sample is hung in rustless steel container 1 interior being used to, sample is positioned at the temperature controlled region of first resistance furnace 3, second resistance furnace 4 is provided with the simple substance sulphur 9 corresponding heating that place the bottom of rustless steel container 1, simple substance sulphur 9 is positioned at the temperature controlled region of second resistance furnace 4, first resistance furnace 3 is provided with first thermopair 7, first thermopair 7 is electrically connected with first temperature controller 5, second resistance furnace 4 is provided with second thermopair, 8, the second thermopairs 8 and is electrically connected with second temperature controller 6.
With reference to Fig. 1, during experiment, temperature with first resistance furnace 3 and second resistance furnace 4 is raised to than high about 100 ℃ of predetermined temperature earlier, then sample is suspended on the stainless steel filament hook 17 below the stainless steel thermofin 11, stainless steel thermofin 11 is put into above the stainless steel stent 10 in the rustless steel container 1 sealing rustless steel container 1, vacuumize and be about 30 minutes, valve-off 13 stops vacuum pump 12, opens argon bottle 15 then and pours into argon gas and be half-full state up to bumping bag 14.Rustless steel container 1 is put into first resistance furnace 3 and second resistance furnace 4, treat to pick up counting when temperature on first temperature controller 5 and second temperature controller 6 is for predetermined temperature.Corrosion finishes, and for preventing that sulphur steam from attached to sample surfaces and rustless steel container 1 upper end, carrying away rustless steel container 1 and putting it at once in the container that fills certain water, the height of the water surface and simple substance sulphur 9 is suitable.After cold the going, take out sample and weigh, after the detection, carry out second and take turns corrosion, up to drawing complete kinetic curve.

Claims (8)

1. high-temperature sulfidation attack experimental provision that is used for material, it is characterized in that: have in the container of cover plate (2) and be provided with support, described support is provided with the filament hook that is used to hang sample, the bottom of described container is placed with the simple substance sulphur (9) of certain mass, described container is connected with one group of vacuum system and one group of argon gas gas charging system, one group of heating system is provided with the corresponding heating of filament hook that sample is hung in interior being used to of described container, and another group heating system is provided with the corresponding heating of simple substance sulphur (9) that place the bottom of described container.
2. the high-temperature sulfidation attack experimental provision that is used for material according to claim 1, it is characterized in that: the top of described support is provided with thermofin.
3. the high-temperature sulfidation attack experimental provision that is used for material according to claim 1 and 2, it is characterized in that: every group of described heating system is made of a temperature controller, a thermopair and a resistance furnace respectively, described temperature controller connects a described thermopair, the described resistance furnace of the corresponding measurement of described thermopair.
4. the high-temperature sulfidation attack experimental provision that is used for material according to claim 1 and 2 is characterized in that: described container is rustless steel container (1).
5. the high-temperature sulfidation attack experimental provision that is used for material according to claim 1 and 2 is characterized in that: described support is stainless steel stent (10).
6. the high-temperature sulfidation attack experimental provision that is used for material according to claim 1 and 2 is characterized in that: described filament hook is stainless steel filament hook (17).
7. the high-temperature sulfidation attack experimental provision that is used for material according to claim 2 is characterized in that: described thermofin is stainless steel thermofin (11).
8. the high-temperature sulfidation attack experimental provision that is used for material according to claim 1 and 2 is characterized in that: described argon gas gas charging system is made up of argon bottle (15) and the bumping bag (14) that is located on the export pipeline of described argon bottle (15).
CN 201010121392 2010-01-20 2010-03-10 Device for high-temperature sulfidation attack experiment of material Pending CN101782497A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201010121392 CN101782497A (en) 2010-01-20 2010-03-10 Device for high-temperature sulfidation attack experiment of material

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201020031430.7 2010-01-20
CN 201010121392 CN101782497A (en) 2010-01-20 2010-03-10 Device for high-temperature sulfidation attack experiment of material

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CN101782497A true CN101782497A (en) 2010-07-21

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103926192A (en) * 2014-03-26 2014-07-16 中国石油化工股份有限公司 Wet sulphur corrosivity testing device for sulphur forming and storage and transportation system and wet sulphur corrosivity testing method
CN104422648A (en) * 2013-08-30 2015-03-18 宝山钢铁股份有限公司 Oil well pipe material deposition sulfur corrosion test method and fixture for sulfur corrosion test
CN104914059A (en) * 2015-06-04 2015-09-16 中国科学院上海应用物理研究所 Absorption spectrometer
CN107643230A (en) * 2017-11-09 2018-01-30 哈尔滨工业大学深圳研究生院 A kind of corrosion rate test equipment under argon gas hot environment
CN107860706A (en) * 2017-12-20 2018-03-30 广电计量检测(北京)有限公司 A kind of sulfidation corrosion experimental rig
CN114324815A (en) * 2021-12-31 2022-04-12 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) High-efficiency accelerated vulcanization comprehensive test device and method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《金属功能材料》 20091215 王辉等 热电池用导电镍带的高温硫化行为研究 15-19 1-8 第16卷, 第6期 2 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104422648A (en) * 2013-08-30 2015-03-18 宝山钢铁股份有限公司 Oil well pipe material deposition sulfur corrosion test method and fixture for sulfur corrosion test
CN104422648B (en) * 2013-08-30 2018-01-30 宝山钢铁股份有限公司 A kind of oil well pipe material deposition sulfur corrosion test method and its test fixture
CN103926192A (en) * 2014-03-26 2014-07-16 中国石油化工股份有限公司 Wet sulphur corrosivity testing device for sulphur forming and storage and transportation system and wet sulphur corrosivity testing method
CN104914059A (en) * 2015-06-04 2015-09-16 中国科学院上海应用物理研究所 Absorption spectrometer
CN107643230A (en) * 2017-11-09 2018-01-30 哈尔滨工业大学深圳研究生院 A kind of corrosion rate test equipment under argon gas hot environment
CN107860706A (en) * 2017-12-20 2018-03-30 广电计量检测(北京)有限公司 A kind of sulfidation corrosion experimental rig
CN114324815A (en) * 2021-12-31 2022-04-12 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) High-efficiency accelerated vulcanization comprehensive test device and method thereof

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Open date: 20100721