CN101905137A - Inner and outer air pressure balanced reaction device of quartz tube - Google Patents
Inner and outer air pressure balanced reaction device of quartz tube Download PDFInfo
- Publication number
- CN101905137A CN101905137A CN2010102362189A CN201010236218A CN101905137A CN 101905137 A CN101905137 A CN 101905137A CN 2010102362189 A CN2010102362189 A CN 2010102362189A CN 201010236218 A CN201010236218 A CN 201010236218A CN 101905137 A CN101905137 A CN 101905137A
- Authority
- CN
- China
- Prior art keywords
- pressure
- quartz tube
- air pressure
- metal shell
- regulating system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention belongs to the technical field of material synthesis, in particular to an inner and outer air pressure balanced reaction device of a quartz tube. The device comprises a metal shell, a metal sealing cover, a gas pipe and a pressure regulating system, wherein the metal shell is connected with the metal sealing cover. The device is characterized in that a through hole is arranged in the metal sealing cover; the inner cavity of the metal shell is internally provided with a sealed quartz tube, and the outer side of the sealed quartz tube is provided with a heater; both ends of the gas pipe are respectively connected with the metal sealing cover and the pressure regulating system; and a pressure gage and a valve are arranged on the gas pipe. The invention has the advantages of simple structure, convenient use, pressure regulation and prevention of high-temperature vacuum collapse and high-inner-pressure bursting of the quartz tube.
Description
Technical field
The invention belongs to field of material synthesis technology, particularly a kind of inner and outer air pressure balanced reaction device of quartz tube.
Background technology
Special experiment condition finds to provide opportunity for the solution and the new physics of many old problems.This is particularly important perfect day by day today at conventional art.Carrying out and the progressive progress of directly depending on experimental technique and device of specific condition research work.
Since quartzy high temperature resistant, corrosion-resistant, easily processing and price are low, carry out so a lot of high temperature synthetic reaction will be encapsulated in material vacuum in the quartz ampoule, as the synthetic synthetic reaction that contains the arsenic iron-based superconductor.Most reactants are to carry out at low pressure with under near the condition of vacuum, and near not occurring subsiding under vacuum, air pressure is lower and temperature is not too high the condition, its reaction can be carried out for a long time as quartz ampoule; If reaction temperature than higher, wants pre-applying argon gas to resist the outer atmospheric pressure of pipe for keeping quartz ampoule not subside usually.
Reactant air pressure in temperature-rise period raises very soon in some synthetic reaction, and quartz ampoule just had explosion danger when air pressure was higher than external atmosphere pressure under the high temperature, made experiment be difficult to carry out even fail.For example when high temperature synthesis iron base superconductor, to use As, Te, materials such as Se participate in pyroreaction.Because these material meeting and metal reactions react so will be placed on the batching sealing in the quartz ampoule.At high temperature air pressure is very high owing to this class material again, so very big air pressure inside causes the quartz ampoule explosion easily, thereby whole experiment is fallen short of success for lack of final effort.Raising as arsenic air pressure when being higher than 600 ℃ can cause the quartz ampoule explosion very soon, takes place for avoiding this class explosion, and reaction temperature can not be too high, this cause again reaction not exclusively or preparation efficiency very low, so just limited temperature, the selection of process parameters scope becomes to grade.
Summary of the invention
Purpose of the present invention be to provide a kind of simple in structure, easy to use, can carry out pressure regulate, prevent the quartz ampoule high-temperature vacuum from subsiding and high in press the inner and outer air pressure balanced reaction device of quartz tube of explosion.
Design of the present invention is to adopt following technical solution to realize: it comprises metal shell, metallic sealed cover, appendix and pressure regulating system, described metal shell is connected with metallic sealed cover, it is characterized in that metallic sealed cover is provided with through hole, be provided with sealed silica envelope in the inner chamber of metal shell, the arranged outside having heaters of sealed silica envelope, the two ends of appendix are connected with pressure regulating system with metallic sealed cover respectively, and appendix is provided with Pressure gauge and valve.
The present invention compared with prior art, owing to adopt in the metal inner cavity of sealing quartz ampoule be set, quartz ampoule arranged outside heater, the structure that pressure regulating system is connected with metal inner cavity through appendix, the pressure reduction that can reach the steam pressure of metal inner cavity pressure and quartz ampoule internal-response deposits yields by the gas pressure of regulating metal inner cavity during use remains in certain scope, realize adjusting the outer air pressure of quartz ampoule so that the pipe inner and outer air pressure is in a basic balance, thereby ensure that sealed silica envelope does not at high temperature subside or explosion, synthetic reaction is normally carried out, it can be widely used in synthesizing under the advanced material specific condition, makes one of ideal device of scientific research and actual production.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is a sealed silica envelope structural representation of the present invention
Drawing reference numeral explanation: 1-metal shell, 2-metallic sealed cover, 3-appendix, 4-Pressure gauge, 5.-valve, 6-pressure regulating system, 7-heater, 8-sealed silica envelope, 9-inner chamber, 10-through hole, 11-vacuum chamber, 12-reactant.
The specific embodiment
With reference to accompanying drawing 1, Fig. 2: the present invention includes metal shell 1, metallic sealed cover 2, appendix 3 and pressure regulating system 6, described metal shell 1 is connected with metallic sealed cover 2, metallic sealed cover 2 is provided with through hole 10, be provided with sealed silica envelope 8 in the inner chamber 9 of metal shell 1, the arranged outside having heaters 7 of sealed silica envelope 8, the two ends of appendix 3 are connected with pressure regulating system 6 with metallic sealed cover 2 respectively, and appendix 3 is provided with Pressure gauge 4 and valve 5; Described gas pressure regulating system 6 adopts the gas boosting power unit of being bought by market, its model is G3032-M-170, described gas pressure regulating system 6 adopts the high pressure manual pump, within its pressure adjustable range 0-50MPa, described heater 7 is buied by market, heater 7 adopts known manner and power supply to join, do not give unnecessary details at this, described heater 7 is used for the heating to sealed silica envelope 8, Pressure gauge 4 can reflect the pressure in the metal inner cavity 9, valve 5 is used for control to metal inner cavity 9 input compressed argon, to regulate the gas pressure in the metal inner cavity 9.
React the former encapsulation employing traditional packaged type of thing in quartz ampoule that drive.In the good reactant 12 of required ratio weighing, then reactant 12 is placed on quartz ampoule 8 bottoms, vacuumize then, after vacuum reaches requirement, utilize torch that quartz ampoule 8 is shut.
In apparatus of the present invention use, with the As that contains for preparing on request, Te, the iron-based superconductor reactant of materials such as Se is placed and is thought in the sealed silica envelope 8, the air pressure of reactant 12 can calculate according to the vapour pressure and the gas equation of heating-up temperature and reactant 12, generally, the sealed silica envelope 8 that wall thickness 1 mm dia is 20 millimeters is adjusted sealed silica envelope 8 outer air pressure so that its pipe inner and outer air pressure is in a basic balance at the inside and outside differential pressure that can bear 1MPa below 1100 degrees centigrade by pressure regulation system 6.
Embodiment:
1, reactant 12 samples that will prepare on request are packaged in the sealed silica envelope 8;
2, sealed silica envelope 8 is put into the heater 7 of metallic cavity 9, then that metallic sealed cover 2 lids are tight;
3, the air pressure that produces according to volatility raw material under sealed silica envelope 8 volumes, gas equation and the material amount experiment with computing temperature;
4, in the process of sample heating, utilize the air pressure in the gas pressure regulating system 6 reacting metal cavitys, make it and to calculate air pressure in a basic balance;
5, test the cooling pressure release that finishes, the blow-on sampling gets final product.
Claims (2)
1. inner and outer air pressure balanced reaction device of quartz tube, comprise metal shell, metallic sealed cover, appendix and pressure regulating system, described metal shell is connected with metallic sealed cover, it is characterized in that metallic sealed cover is provided with through hole, be provided with sealed silica envelope in the inner chamber of metal shell, the arranged outside having heaters of sealed silica envelope, the two ends of appendix are connected with pressure regulating system with metallic sealed cover respectively, and appendix is provided with Pressure gauge and valve.
2. inner and outer air pressure balanced reaction device of quartz tube according to claim 1 is characterized in that described gas pressure regulating system adopts the gas boosting power unit, and its model is G3032-M-170, within its pressure adjustable range 0-50MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010236218.9A CN101905137B (en) | 2010-07-26 | 2010-07-26 | Inner and outer air pressure balanced reaction device of quartz tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010236218.9A CN101905137B (en) | 2010-07-26 | 2010-07-26 | Inner and outer air pressure balanced reaction device of quartz tube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101905137A true CN101905137A (en) | 2010-12-08 |
| CN101905137B CN101905137B (en) | 2015-10-14 |
Family
ID=43260812
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010236218.9A Expired - Fee Related CN101905137B (en) | 2010-07-26 | 2010-07-26 | Inner and outer air pressure balanced reaction device of quartz tube |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101905137B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757360A (en) * | 2016-12-27 | 2017-05-31 | 珠海鼎泰芯源晶体有限公司 | The horizontal synthesizer of indium phosphide polycrystal and control method for pressure balance |
| CN107747125A (en) * | 2017-09-20 | 2018-03-02 | 广东先导先进材料股份有限公司 | The pressure control device and method of indium phosphide polycrystal synthesis |
| CN113035748A (en) * | 2021-02-27 | 2021-06-25 | 楚赟精工科技(上海)有限公司 | Vacuum chamber, pressure control method thereof, and semiconductor processing apparatus |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4059145A (en) * | 1975-06-05 | 1977-11-22 | Sid Richardson Carbon & Gasoline Co. | Method and apparatus for controlling surface temperature |
| CN1744942A (en) * | 2002-01-31 | 2006-03-08 | 通用电气公司 | Improved pressure vessel |
| CN101163540A (en) * | 2005-01-25 | 2008-04-16 | 通用电气公司 | Apparatus for processing materials in supercritical fluids and methods thereof |
-
2010
- 2010-07-26 CN CN201010236218.9A patent/CN101905137B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4059145A (en) * | 1975-06-05 | 1977-11-22 | Sid Richardson Carbon & Gasoline Co. | Method and apparatus for controlling surface temperature |
| CN1744942A (en) * | 2002-01-31 | 2006-03-08 | 通用电气公司 | Improved pressure vessel |
| CN101163540A (en) * | 2005-01-25 | 2008-04-16 | 通用电气公司 | Apparatus for processing materials in supercritical fluids and methods thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757360A (en) * | 2016-12-27 | 2017-05-31 | 珠海鼎泰芯源晶体有限公司 | The horizontal synthesizer of indium phosphide polycrystal and control method for pressure balance |
| CN106757360B (en) * | 2016-12-27 | 2023-10-03 | 珠海鼎泰芯源晶体有限公司 | Indium phosphide polycrystal horizontal synthesis device and pressure balance control method |
| CN107747125A (en) * | 2017-09-20 | 2018-03-02 | 广东先导先进材料股份有限公司 | The pressure control device and method of indium phosphide polycrystal synthesis |
| CN113035748A (en) * | 2021-02-27 | 2021-06-25 | 楚赟精工科技(上海)有限公司 | Vacuum chamber, pressure control method thereof, and semiconductor processing apparatus |
| CN113035748B (en) * | 2021-02-27 | 2022-03-11 | 楚赟精工科技(上海)有限公司 | Vacuum chamber, pressure control method thereof, and semiconductor processing apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101905137B (en) | 2015-10-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN206082526U (en) | Reaction kettle with gas -assisted stirring mechanism | |
| CN101498638B (en) | Test device for weight change of pressurized high-temperature solid example and use thereof | |
| CN104004958A (en) | Method and device for continuously preparing vanadium-nitrogen alloy | |
| CN101905137A (en) | Inner and outer air pressure balanced reaction device of quartz tube | |
| CA2909776A1 (en) | Systems and methods of making ammonia using hydrogen and nitrogen gases | |
| CN210115062U (en) | Self-balancing dropwise add reation kettle | |
| Hougen et al. | Reduction of tungsten oxides with hydrogen | |
| CN204989081U (en) | Device of fuel factor among warm reaction sequence such as measurement carbon macromolecule | |
| CN206587738U (en) | A kind of vacuum high-temperature closed reactor | |
| CN202212158U (en) | Reaction kettle for pickling high-purity quartz sand | |
| CN206362178U (en) | A kind of vacuum synthesis stove | |
| CN201701766U (en) | Heat-conducting oil level control device of clamping sleeve | |
| CN111398348A (en) | Natural gas amine decarburization reaction heat measurement system based on adiabatic calorimetry and reaction heat measurement method | |
| CN202415149U (en) | Intelligent type in vitro heating high-purity chlorine dioxide generator adopting chemical sodium chlorate method | |
| CN105170058B (en) | A kind of quick microwave plasma reaction unit for preparing material | |
| CN204147835U (en) | Solid reaction still | |
| CN208617360U (en) | A kind of device preparing hydrogen fluoride by fluosilicic acid | |
| CN201684604U (en) | Pre-exhaust device of heat pipe working medium reactor | |
| CN201592079U (en) | Reactor for preparing antimony pentafluoride | |
| CN202219163U (en) | Temperature control device for EPS (expandable polystyrene) reaction kettle | |
| CN202078893U (en) | Two-temperature-zone synthesizing vessel and device for P-group polynary compounds | |
| CN207662670U (en) | A kind of valeronitrile hydrogenation pressure autoclave type sampling jar | |
| CN204338132U (en) | A kind of reactor device for saponin open loop | |
| CN207468725U (en) | A kind of high-purity gas cylinder inner wall MOCVD nickel plating apparatus | |
| CN207254291U (en) | A kind of pickling high-purity quartz sand reaction kettle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151014 Termination date: 20160726 |