CN109246860A - In situ, dynamic observation material high temperature service under the microscope can be achieved - Google Patents

In situ, dynamic observation material high temperature service under the microscope can be achieved Download PDF

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Publication number
CN109246860A
CN109246860A CN201811136644.8A CN201811136644A CN109246860A CN 109246860 A CN109246860 A CN 109246860A CN 201811136644 A CN201811136644 A CN 201811136644A CN 109246860 A CN109246860 A CN 109246860A
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CN
China
Prior art keywords
chamber
microscope
situ
unit
temperature service
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Pending
Application number
CN201811136644.8A
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Chinese (zh)
Inventor
谢伟广
曾文
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Jinan University
University of Jinan
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Jinan University
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Publication date
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Priority to CN201811136644.8A priority Critical patent/CN109246860A/en
Publication of CN109246860A publication Critical patent/CN109246860A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/24Base structure
    • G02B21/30Base structure with heating device
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/34Microscope slides, e.g. mounting specimens on microscope slides

Abstract

In situ, dynamic observation material high temperature service under the microscope can be achieved the invention discloses a kind of.The high temperature service includes main cavity, is set to the intracorporal inner chamber body of main chamber, heating unit, ventilation unit and vacuum unit;The window for observation is provided on main cavity;Heating unit, ventilation unit and vacuum unit are connect with inner chamber body respectively;Heating unit is used to provide hot environment for inner chamber body;Ventilation unit is used to ventilate for inner chamber body;Vacuum unit is for vacuumizing inner chamber body.The high temperature service is small in size, is able to satisfy high temperature, ventilation and the vacuum condition of Material growth, is equipped with watch window, can observe the high temperature dynamic process of material under the microscope.

Description

In situ, dynamic observation material high temperature service under the microscope can be achieved
Technical field
The present invention relates to investigation of materials and in situ detection fields, in particular to a kind of achievable in situ under the microscope, dynamic The high temperature service of state observation material.
Background technique
As modern microelectronic and optoelectronics industry are towards integrated and miniaturization trend, material science gradually at For a research material technology of preparing, growth mechanism, control method and Physical Property Analysis science.Growth, phase transformation of material etc. are dynamic The research of state process is to control the essential step of material property.The characteristics such as structure, the pattern of material have emphatically the performance of material The influence wanted;Only understand the dynamic processes such as growth, the phase transformation of material in depth, it could be to its structure, pattern and correlation properties It is precisely controlled;Therefore, the research for furtheing investigate MATERIALS ' DYNAMIC process has great directive significance to investigation of materials.
But detection and observation device are limited by for the research of material in situ process at present;To Material growth process Research be to be carried out under conditions of closed mostly, can only be speculated by ex-post analysis growth morphology and crystal quality influence because Element.By taking prepared by material as an example, the environment of most thin-film material growth can not carry out home position observation.Such as using vacuum vapour deposition, The film of the methods of magnetron sputtering method and solwution method preparation is mostly continuous noncrystal membrane, needs to make annealing treatment in tube furnace Nano particle, nanometer sheet, nanometer rods or continuous polycrystal film can just be grown into.Due to the special growing environment of tube furnace And structure, we can not be by itself and microscope combination progress home position observation Material growth process.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies and insufficient, provide it is a kind of can be achieved it is former under the microscope Position, dynamic observation material high temperature service, the high temperature service is small in size, is able to satisfy high temperature, ventilation and the vacuum of Material growth Condition is equipped with watch window, can observe the high temperature dynamic process of material under the microscope.
The purpose of the present invention can be achieved through the following technical solutions:
It can be achieved in situ, dynamic observation material high temperature service under the microscope, including main cavity, be set in main cavity Inner chamber body, heating unit, ventilation unit and vacuum unit;The window for observation is provided on main cavity;Heating is single Member, ventilation unit and vacuum unit are connect with inner chamber body respectively;Heating unit is used to provide hot environment for inner chamber body;It is logical Gas unit is used to ventilate for inner chamber body;Vacuum unit is for vacuumizing inner chamber body.
Heating unit includes copper electrode, resistor disc fixture block and resistor disc, two pieces of copper electrodes as a preferred technical solution, It is connected to the resistor disc fixture block positioned at inner chamber body by the two sides of main cavity, resistor disc is fixed by two pieces of resistor disc fixture blocks.
Copper electrode is separated with main cavity contact position with polytetrafluoroethylene (PTFE) interlayer as a preferred technical solution,.Polytetrafluoroethyl-ne Alkene interlayer separates main cavity and copper electrode, plays insulation, sealing and heat-insulated effect.
Resistor disc is that tantalum piece, leaf or height lead silicon wafer as a preferred technical solution, and resistance range is 0.1 Ω -1 Ω.Electricity Resistance piece can provide the high temperature higher than 1000 DEG C for investigation of materials.
Ventilation unit is snorkel as a preferred technical solution, and snorkel one end connects inner chamber body, and the other end is equipped with method Blue interface, for connecting external feeder.
The logical gas of ventilation unit is nitrogen or argon gas or oxygen or hydrogen as a preferred technical solution,.Ventilation unit Ventilated body can be not limited to above-mentioned listed gas, can also lead to other gases according to Material growth needs.
Vacuum unit is exhaust tube as a preferred technical solution, and exhaust tube one end connects inner chamber body, and the other end is equipped with Two flange-interfaces are respectively used to connection vacuum pump and vacuum meter.Vacuum pump is used to inner chamber body being evacuated to vacuum, and vacuum meter is used for Measure the intracorporal vacuum degree in inner cavity.
High temperature service further includes temperature detecting unit as a preferred technical solution, and temperature detecting unit includes that aviation connects Head and thermocouple, Aviation Connector penetrate through main cavity, and thermocouple passes through Aviation Connector and accesses inner chamber body.Temperature detecting unit can The intracorporal temperature in inner cavity is detected, accurately controls the intracorporal temperature change in inner cavity in conjunction with heating power supply.
Cooling water channel is equipped between main cavity and inner chamber body as a preferred technical solution, is set in main cavity side wall surface There is cooling water outlet and inlet.When cooling water channel can reduce resistor disc work, heat is to main cavity externalities, it is ensured that main cavity External temperature is maintained at 22 DEG C or so.
Main cavity bottom is connected with detachable support plate as a preferred technical solution,.Detachable support plate, which facilitates, fills high temperature It sets and is fixed on microscope carrier.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1, heating unit, ventilation unit and the vacuum unit in the present invention can be needed for accurate controlled material growths The conditions such as temperature, throughput and pressure can meet the material for needing high temperature, high vacuum and gas assisting growth condition, fit It makes annealing treatment and grows for various precursor thin films.
2, watch window is equipped in the present invention, can observe, pattern of the recording materials from solid film to crystallization process, at Point variation, can home position observation material under the microscope dynamic growth process.
3, high temperature service of the invention is small in size, and heating efficiency is high, and most of part is detachable, facilitate transfer, carry with And Function Extension.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of high temperature device of the embodiment of the present invention
Fig. 2 is the bottom view of Fig. 1
Fig. 3 is the structural schematic diagram of heating unit in the embodiment of the present invention
Fig. 4 is that resistor disc temperature controls I-T curve graph in the embodiment of the present invention
Wherein: 1- exhaust tube;2- flange-interface;3- inner chamber body;4- glass gland;5- snorkel;6- main cavity;7- poly- four Vinyl fluoride interlayer;8- copper electrode;The detachable support plate of 9-;10- watch window;11- resistor disc fixture block;12- resistor disc;13- is cooling Water entrance;14- aviation interface;15- screw recess;16- cooling water channel;17- screw through-hole.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited In this.
As shown in Figure 1, being provided in the embodiment of the present invention a kind of achievable in situ under the microscope, dynamic observation material High temperature service, including main cavity 6, inner chamber body 3, heating unit, ventilation unit and vacuum unit.Heating unit, ventilation are single Member and vacuum unit are connect with inner chamber body 3 respectively, provide required temperature, gas and pressure conditions for sample grown.
Main cavity 6 is the main body frame of high temperature service, is the small cube of 80mm × 80mm × 43mm, by high duty metal system It makes, it being capable of high temperature high voltage resistant.Inner chamber body 3 is set to inside main cavity 6, is a cylindrical body of middle part hollow out, is provided for material Growing space.Watch window 10 is provided with above inner chamber body 3, watch window 10 is one block of quartz glass, and quartz glass seals are lived The upper port of inner chamber body 3.Quartz glass is fixed by the glass gland 4 above it.Quartz glass has high transparency, high temperature resistant And the characteristics of high rigidity, micro objective optical path can be placed on resistor disc 12 by quartz glass, sample, microscope Observable The growth course of sample is recorded.
As shown in figure 3, heating unit includes copper electrode 8, resistor disc fixture block 11 and resistor disc 12, two pieces of copper electrodes 8 are logical Two side through hole for crossing main cavity 6 are connected to resistor disc fixture block 11 positioned at inner chamber body 3, and resistor disc 12 is by two pieces of resistor disc fixture blocks 11 It is fixed.Resistor disc 12 is high-temperature electric conduction material, and tantalum piece, leaf or height can be selected and lead silicon wafer etc., and resistance range is 0.1 Ω -1 Ω, The high temperature provided higher than 1000 DEG C can be studied for sample.By external heating power supply to copper electrode 8 plus electric current, it can be achieved that resistor disc 12 accurate heating, to provide hot conditions for sample grown.Copper electrode 8 and 6 contact position polytetrafluoroethylene (PTFE) of main cavity every Layer 7 separates.Polytetrafluoroethylene (PTFE) interlayer 7 plays insulation, sealing and heat-insulated effect.
In order to detect the temperature inside high temperature service, high temperature service further includes temperature detecting unit.Temperature detecting unit packet Include Aviation Connector 14 and thermocouple.By the through-hole on 6 side of main cavity, thermocouple passes through Aviation Connector and connects Aviation Connector Enter inner chamber body 3, the tip temperature sensing point top to the bottom of resistor disc 12 of thermocouple.The 14 external connection temperature control of aviation interface is shown Meter, can accurately show the precision of the temperature to 0.1 DEG C of resistor disc 12.Heating power supply is used cooperatively with temperature control display meter, can be passed through The setting of automated intelligent temperature control is realized in programming.Fig. 4 is resistor disc temperature control I-T curve graph, the heating temperature and heating of resistor disc The current squaring of power supply is directly proportional, this meets Joule's law.I.e. by adjusting the electric current of heating power supply, then can accurately control The temperature of resistor disc.
Ventilation unit is snorkel 5.The diameter of snorkel 5 is 6mm, and outside port is equipped with KF16 flange-interface 2, for connecting Connect external air feed equipment.Gas needed for snorkel 5 is passed through sample grown, such as oxygen, argon gas.Inner cavity is adjusted in ventilation unit Pressure inside body 3.
Pumping cells are exhaust tube 1.Exhaust tube 1 is passed through from main cavity 6, is passed through inner chamber body 3.Exhaust tube 1 is by diameter The pumping pipeline section and diameter of 10mm is that pumping pipeline section two parts T of 16mm connects composition.Pumping pipeline section and the master that diameter is 10mm Cavity 6 connects, and end is steeved upwards horizontal by 45° angle, is conducive to 1 upper flange interface 2 of exhaust tube connection external equipment.Directly The pumping pipeline section that diameter is 16mm is connect with the end for the pumping pipeline section that diameter is 10mm, and both ends are equipped with KF16 flange-interface 2.One end Flange-interface 2 connect vacuum pump, such as connection standard machinery pump the air pressure in inner chamber body 3 can be evacuated to 10 by exhaust tube 1- 2Pa.The flange-interface 2 of the other end connects resistance vacuum gauge, for detecting the vacuum degree of inner chamber body 3.
Influence of the high temperature generated when inner chamber body 3 works in order to prevent to main cavity 6 and external device (ED), outside main cavity 6 Wall surface between 3 inner wall of inner chamber body be equipped with cooling water channel 16.As shown in Fig. 2, cooling water channel 16 is in U-typed, main cavity 6 is covered Most of region.Cooling water outlet and inlet 13 there are two being set at the corresponding position in U-typed head of cooling water channel 16.Cooling water into 13 external cooling water tanks are exported, after being passed through cooling water, it is ensured that 6 external temperature of main cavity maintains 22 DEG C or so.It is cold to avoid But water leaks out, the sealed bottom of main cavity 6.
High temperature service is placed under microscope for convenience, one piece of detachable support plate 9 is installed in 6 bottom of main cavity. According to Golden Elephant WSM800BD-G model microscope carrier, the specification of detachable support plate 9 is 220mm × 220mm × 4mm, material For steel plate.Screw recess 15 is neatly equipped on detachable support plate 9,6 bottom of main cavity is equipped with 4 screw through-holes 17, passes through screw It can be fixed by detachable support plate 9 and main cavity 6.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (10)

1. in situ, dynamic observation material high temperature service under the microscope can be realized, which is characterized in that including main cavity, setting In the intracorporal inner chamber body of main chamber, heating unit, ventilation unit and vacuum unit;It is provided on main chamber body for observing Window;The heating unit, ventilation unit and vacuum unit are connect with the inner chamber body respectively;The heating unit is used In providing hot environment for inner chamber body;The ventilation unit is used to ventilate for inner chamber body;The vacuum unit is used for inner cavity Body vacuumizes.
2. in situ, dynamic observation material high temperature service, the feature according to claim 1 under the microscope of can be achieved exists In the heating unit includes copper electrode, resistor disc fixture block and resistor disc, the two sides that two pieces of copper electrodes pass through main cavity It is connected to the resistor disc fixture block positioned at inner chamber body, the resistor disc is fixed by two pieces of resistor disc fixture blocks.
3. in situ, dynamic observation material high temperature service, the feature according to claim 2 under the microscope of can be achieved exists In the copper electrode is separated with main cavity contact position with polytetrafluoroethylene (PTFE) interlayer.
4. in situ, dynamic observation material high temperature service, the feature according to claim 2 under the microscope of can be achieved exists In the resistor disc is that tantalum piece, leaf or height lead silicon wafer, and resistance range is 0.1 Ω -1 Ω.
5. in situ, dynamic observation material high temperature service, the feature according to claim 1 under the microscope of can be achieved exists In the ventilation unit is snorkel, and described snorkel one end connects inner chamber body, and the other end is equipped with flange-interface, for connecting External feeder.
6. in situ, dynamic observation material high temperature service under the microscope can be realized according to claim 1 or 5, it is special Sign is that the logical gas of the ventilation unit is nitrogen or argon gas or oxygen or hydrogen.
7. in situ, dynamic observation material high temperature service, the feature according to claim 1 under the microscope of can be achieved exists In, the vacuum unit is exhaust tube, and described exhaust tube one end connects inner chamber body, and the other end is set there are two flange-interface, point Vacuum pump and vacuum meter Yong Yu not connected.
8. in situ, dynamic observation material high temperature service, the feature according to claim 1 under the microscope of can be achieved exists In the high temperature service further includes temperature detecting unit, and the temperature detecting unit includes Aviation Connector and thermocouple, described Aviation Connector penetrates through main chamber body, and the thermocouple is by the Aviation Connector and accesses inner chamber body.
9. in situ, dynamic observation material high temperature service, the feature according to claim 1 under the microscope of can be achieved exists In equipped with cooling water channel between main chamber body and the inner chamber body, equipped with cooling water disengaging on the wall surface of main chamber side Mouthful.
10. according to claim 1 can be achieved in situ, dynamic observation material high temperature service under the microscope, feature It is, main chamber body bottom is connected with detachable support plate.
CN201811136644.8A 2018-09-28 2018-09-28 In situ, dynamic observation material high temperature service under the microscope can be achieved Pending CN109246860A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111198154A (en) * 2020-01-08 2020-05-26 同济大学 Visual testing arrangement of fuel cell metal bipolar plate continuous corrosion
CN112034609A (en) * 2020-11-04 2020-12-04 成都泰盟软件有限公司 Novel animal mesentery microcirculation observation device

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Publication number Priority date Publication date Assignee Title
CN2388611Y (en) * 1999-06-15 2000-07-19 中国洛阳浮法玻璃集团有限责任公司 High-temp. microscope heating stand
US20060053652A1 (en) * 2002-11-21 2006-03-16 Gyory J R Freeze-drying microscope stage apparatus and process of using the same
CN101839846A (en) * 2010-05-07 2010-09-22 上海工程技术大学 High-resolution high-temperature metallographic structure analyzer
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111198154A (en) * 2020-01-08 2020-05-26 同济大学 Visual testing arrangement of fuel cell metal bipolar plate continuous corrosion
CN112034609A (en) * 2020-11-04 2020-12-04 成都泰盟软件有限公司 Novel animal mesentery microcirculation observation device

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