CN107727697A - A kind of probe in-situ resistivity-measuring devices of high flux material chip four - Google Patents
A kind of probe in-situ resistivity-measuring devices of high flux material chip four Download PDFInfo
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- CN107727697A CN107727697A CN201711019802.7A CN201711019802A CN107727697A CN 107727697 A CN107727697 A CN 107727697A CN 201711019802 A CN201711019802 A CN 201711019802A CN 107727697 A CN107727697 A CN 107727697A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/14—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature
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Abstract
The present invention provides a kind of probe in-situ resistivity-measuring devices of high flux material chip four, belongs to Material Testing Technology field.The equipment includes the probe of high flux four, the airtight tank body of high temperature high voltage resistant, sample pallet, the probe instrument of multichannel four, transmission cable and data logging software；Sample pallet is located in high temperature high voltage resistant tight tank body, the probe of high flux four is arranged on sample pallet, the probe of high flux four passes through the probe instrument of transmission cable connecting multi-channel four, data logging software is installed on host computer, receives the data from the measurement of the probe instrument of multichannel four.The present invention can be under high temperature and high pressure gas environment, four probe resistances of up to 64 samples are measured and recorded simultaneously with the change of the parameters such as time, air pressure, temperature, possess enough precision and reliability, high data acquiring frequency, cheap hardware cost and shirtsleeve operation method, while the requirement accurately measured a small amount of sample resistance can also be met.
Description
Technical field
The present invention relates to Material Testing Technology field, particularly relates to a kind of probe in-situ resistance of high flux material chip four and surveys
Measure equipment.
Background technology
Material high flux experimental method in material genome plan, it is a kind of efficient new material research and development method.Its core
Thought thinks it is preparation and the sign for completing lot of materials sample in a short time, and therefrom filters out the sample for meeting performance requirement
Corresponding corresponding technique.Compared to traditional " trial-and-error method ", high throughput test method has that the R＆D cycle is short, development cost are low, personnel
The advantages such as labor intensity is low, it is the cutting edge technology of present material scientific research and application field development.
Combination of materials chip technology is a kind of method that high flux prepares lot of materials sample, and its general thinking is to use
PVD equipment, using discrete mask plate method either cosputtering method by a large amount of binary with heterogeneity, ternary or how far material
It is prepared on one piece of small substrate, the flux for the lifting sample preparation that this method can be high.And high flux is carried out to these samples
Sign and test, then demand is proposed to high-throughout Materials Measurement technology.
Basic physical attribute of the resistance as material, in novel semiconductor material, dielectric material, battery material, magnetic material
Occupy critical role in the research and development of material etc..In addition, in the research of some gas sensor materials, it is also desirable to measure resistance with gas
The variation relation of bulk concentration and temperature, just the in site measurement to resistance and recording technique propose requirement for this.By high flux resistance
E measurement technology is combined with the combined chip technology of preparing of material, the purpose for preparing and detecting with regard to that can reach high flux material.Tradition
Electric resistance measuring apparatus to reach this purpose, usually using the probe of step motor control, measure the electricity of regional successively
Resistance, but be so difficult to meet in site measurement and the requirement of record, particularly in the harsh environment of HTHP, work as needs in addition
It is long to the measurement interval of each sample, it is difficult to tackle the fast-changing situation of resistance during the resistance variations of continuous record sample.
In addition, four-point probe table domestic commercial at present is mostly single channel, separate unit Meter cost generally more than 5000 yuan, if
Not only with high costs for high flux resistance measurement, there is also the problem of line complexity.The present invention uses the design of integration,
For the application problem of material high flux resistance in site measurement, there is provided it is a set of aim at material high flux research and development in resistance in high temperature height
The in site measurement of pressure ring border and the device of record, there is simple to operate, relative inexpensiveness, stable and reliable operation, measurement essence
The advantages of degree is high, data record amount is big, it compensate for the blank of the domestic field application technology.
The content of the invention
The present invention is directed to high flux material development, there is provided a kind of probe in-situ resistance measurement of high flux material chip four is set
It is standby, it is applicable not only to original position electricity of the high flux material sample of combination of materials chip method preparation in HTHP harsh environment
Resistance measurement record, can also meet the needs of a small amount of resistance accurately measures simultaneously.
The equipment includes the probe of high flux four, the airtight tank body of high temperature high voltage resistant, sample pallet, the probe of multichannel four electricity
Hinder tester, transmission cable and data logging software；Sample pallet is located in high temperature high voltage resistant tight tank body, the probe of high flux four
Probe is arranged on sample pallet, the probe of high flux four by the probe instrument of transmission cable connecting multi-channel four,
Data logging software is installed on host computer, and data logging software receives the number from the measurement of the probe instrument of multichannel four
According to, and carry out real-time display and record.
Wherein, the airtight tank body of high temperature high voltage resistant is used to provide the pressure and atmosphere needed for reaction, by top cover labyrinth to resistance to
The airtight tank body of HTHP is sealed；The airtight tank body of high temperature high voltage resistant uses high-class stainless steel material, internally no more than 500
DEG C and 6MPa pressure under conditions of use, noncorrosive gases such as hydrogen, oxygen, carbon monoxide, methane etc. are in high temperature high voltage resistant
Reacted in tight tank body with sample.
The airtight tank body of high temperature high voltage resistant is provided with electric coupler part, for the high flux in high temperature high voltage resistant tight tank body
The cable of the cable of four probes and the outside probe instrument of multichannel four is attached, and can complete electric signal transmission
Ensure that tank body is air tight while task；Top cover labyrinth is provided with air pressure and temperature instrument, and is alarmed provided with over-pressure over-temperature
Component and relief valve, urgent exhaust passage is additionally provided with, it is airtight that emergency exhausting pipe road can empty high temperature high voltage resistant within 1~3s
Gas in tank body, ensures safety in utilization to greatest extent.
The probe of high flux four includes shell, fixed knob, cable jointing and probe, the probe of high flux four
Buffer unit built in probe, it is scalable pattern for installing the probe directly contacted with sample, can be non-hard with sample surfaces
Property contact, probe spacing fixed, contacted based on vanderburg method principle with each sample, and being mainly used in measurement, there are gradient components to be distributed
Film sample (being also known as material chip)；Cable jointing is located in shell, and fixed knob is used for the probe of high flux four
Probe is fixed with sample pallet.
Transmission cable inner lead is high temperature resistant material, and all using twisted-pair feeder shielding processing.
Sample pallet uses monolithic construction, can adjust after loading sample and fixes sample position, in favor of on probe
Probe is strictly aligned with each sample, is fixed between probe and specimen holder using bolt, and adjustable relative distance is visited so as to change
The contact force size of pin and sample surfaces.Resistance heating device and Temperature-controlled appliance are provided with inside sample pallet, by resistance to height
Switching Power Supply power supply outside the warm airtight tank body of high pressure；Sample pallet includes interface, knob, pedestal and fixture, interface, knob and
Fixture is located on pedestal, and interface is used to be connected with the probe of high flux four, and knob is used to adjust sample position, and fixture is used to adjust
Section and fixed sample position.
The probe instrument of multichannel four uses integral structure, has been internally integrated in a shell structure logical including 64
The voltage-controlled constant-current supply module of the high accuracy for being independently arranged constant current size in road, microprocessor control module, 64 passages electricity
Press sample circuit and high-precision degree type ADC, temperature detecting module, communication module, peripheral interface circuit and switch power module；
Set outside the probe instrument of multichannel four joint, four pin data-interfaces, LCD display, measurement pattern selecting switch,
LCD brightness regulation knobs and total power switch, joint are used to complete data input output with transmission cable, and four pin data-interfaces are
The binding post of 1~8 passage, the sample frequency of each passage are set in data logging software, and highest sample frequency exceedes
50 times/second.In terms of peripheral interface, instrument has reserved two special purpose interfaces, has been respectively used to provide electricity for the probe of high flux four
Hinder the output of measuring constant-current supply and gather the voltage signal input of multiple passages, only need to be by the plug of client cables during use
Two interfaces are respectively connected to, effectively prevent wiring error and the bad influence to experiment of wiring circuit contact, while greatly
Reduce labor intensity.In addition to the application of high flux resistance test, the instrument has also reserved the binding post of 1~8 passage,
Can meet the needs of testing to a small amount of probe resistance of sample four.The instrument reserved RS485 and TCP/IP interfaces be used for it is upper
Machine communicates.In addition, the equipment can be autonomous to select constant-current source output valve to obtain size according to measured resistance scope automatic switching range,
And the work between each passage is separate.
Current resistive value that data logging software real-time display measures and resistance value with the time, air pressure, temperature change song
Line, data are exported in the form of Excel or txt text document files.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
The complete set of equipments that the present invention designs, sample are placed on the sample stage with temperature function and probe fixing function,
The accurate alignment and the control of accurate sample temperature, HTHP hermetically sealed can that probe can be ensured provide safe survey for sample
Test ring border, special signal transmission cable make experiment assembling and connection procedure simple and convenient, and the high flux resistance of autonomous Design is surveyed
Examination instrument can coordinate probe to realize the up to purpose of 64 probe resistance of sample four measurements and record, data logging software interface friend
It is good, more can be powerful, it is easy to use.The equipment designs for high flux experimental applications, while can also meet daily a small amount of sample
Resistance test demand, while relative inexpensiveness, good reliability, there is wide application model in the high flux research field of material
Enclose.
Brief description of the drawings
Fig. 1 is the probe in-situ resistivity-measuring devices structural representation of high flux material chip four of the present invention；
Fig. 2 is the probe instrument structural representation of multichannel four of the independent research of the present invention；
Fig. 3 is the sample pallet structural representation with temperature control function of the present invention；
Fig. 4 is the probe structural representation of high flux four of the present invention.
Wherein：1- includes the probe of high flux four；The airtight tank body of 2- high temperature high voltage resistants；3- sample pallets；Sealed on 4-
Lid；5- transmission cables；The probe instrument of 6- multichannels four；7- data logging softwares；11- shells；12- fixed knobs；13-
Cable jointing；14- probes；31- interfaces；32- knobs；33- pedestals；34- fixtures；61- joints；The pin data-interfaces of 62- tetra-；
63-LCD display screens；64- measurement pattern selecting switch；65-LCD brightness regulation knobs；66- total power switch.
Embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of probe in-situ resistivity-measuring devices of high flux material chip four.
As shown in figure 1, being the device structure schematic diagram, in the equipment, sample pallet 3 is located at the airtight tank body of high temperature high voltage resistant
In 2, the probe 1 of high flux four is arranged on sample pallet 3, and the probe 1 of high flux four is connected more logical by transmission cable 5
The probe instrument 6 of road four, data logging software 7 are installed on host computer, and data logging software 7 is received and visited from multichannel four
The data that pin resistance meter 6 measures, and carry out real-time display and record.
As shown in Fig. 2 the probe instrument 6 of multichannel four uses integral structure, collect inside a shell structure
Into the voltage-controlled constant-current supply module of the high accuracy for being independently arranged constant current size, the microprocessor control mould for including 64 passages
Block, 64 channel voltage sample circuits and high-precision degree type ADC, temperature detecting module, communication module, peripheral interface circuit and open
Powered-down source module；The outside of four probe instrument of multichannel 6 set joint 61, four pin data-interfaces 62, LCD display 63,
Measurement pattern selecting switch 64, LCD brightness regulation knobs 65 and total power switch 66, joint 61 are used to complete number with transmission cable
According to input and output, four pin data-interfaces 62 are the binding post of 1~8 passage, and the sample frequency of each passage is in data record
Set in software 7, highest sample frequency is more than 50 times/second.
As shown in figure 3, sample pallet 3 uses monolithic construction, the inside of sample pallet 3 is provided with resistance heating device and temperature
Control device is spent, is powered by the Switching Power Supply outside the airtight tank body 2 of high temperature high voltage resistant；Sample pallet 3 includes interface 31, knob
32nd, pedestal 33 and fixture 34, interface 31, knob 32 and fixture 34 are located on pedestal 33, and interface 31 is used for and the probe of high flux four
The connection of probe 1, knob 32 are used to adjust sample position, and fixture 34 is used to adjusting and fixing sample position.
As shown in figure 4, the probe 1 of high flux four includes shell 11, fixed knob 12, cable jointing 13 and probe
14, the probe 1 of high flux four is used to install the probe 14 directly contacted with sample, buffer unit built in probe 14, Neng Gouyu
The non-rigid contact of sample surfaces, the spacing of probe 14 are fixed；Cable jointing 13 is located in shell 11, and fixed knob 12 is used for height
The probe 1 of flux four is fixed with sample pallet 3.
In actual use, contain 64 kinds of heterogeneities by prepared by combination of materials chip technology first, be deposited on
Film sample on same non-conductive substrate, it is put into sample pallet sample room as shown in Figure 2, adjusts good position and clamp
It is good.
, will probe and specimen holder with bolt by the sound end alignment sample side of the probe of high flux four shown in Fig. 3
Platform connects, and because sample is using matching mask plate preparation, and sample has adjusted good position and clamped, therefore on probe
Each probe can be contacted just with sample, and meet vanderburg method measurement resistance principle probe is just contacted with sample edge
Requirement.
The opposite side of the probe of high flux four is equipped with a plug to be drawn by dedicated transmissions cable, by the plug
It is connected with inside the electrical connector of airtight tank body.Then the top cover labyrinth of airtight tank body is covered, is tightened using supporting bolt, and
Carry out gas leak detection operation.
By two plugs of external dedicated transmission cable respectively with it is outside the electrical connector of airtight tank body and as shown in Figure 2
The probe resistance measuring instrument of multichannel four input and output special purpose interface connection.
The probe resistance measuring instrument of multichannel four is connected with host computer using the RS485 order wires of standard, opens multichannel
The power switch of four probe resistance measuring instruments, preheat 20min.Then the data record for the independent development installed in host computer is opened
Software, each passage of sample of required measurement is configured.Configuration content includes：Can be according to the substantially resistance range of each sample
The surveying range of instrument is set manually, and now instrument can configure the size of current that constant-current source exports according to the scope of measured resistance value
With the multiplication factor of voltage collection circuit operational amplifier, also may be selected can be in testing according to first without configuration, system
The resistance value dynamic adjustment relevant parameter measured.Select the time interval of each channel data record, i.e. sample frequency.The survey of software
Die trial formula is divided into three classes：" when m- resistance ", " temperature-resistance ", " gas piezo-resistive ", unless separately setting, system will be given tacit consent to
For " when m- resistance " pattern, using resistance as ordinate, the time is that abscissa carries out lasting data record, is stopped until pressing
Record button.If being configured to other both of which, respectively using temperature or air pressure as abscissa, the non-ordinate of resistance is remembered
Record, and software also provides option：" the record time is the second abscissa ", the time if desired is recorded simultaneously, then in this final election
Frame is lower to make hook, and now software can be recorded in measurement process by the second abscissa of the time, and otherwise software measures again
During will not record the time.After configuration, you can start resistance measurement and the data recording function of whole equipment.
The test environment of sample is selected, if desired measures sample resistance variation with temperature relation, can configure in hermetically sealed can
Sample holder temperature control device corresponds to controller, sets initial temperature, the step-length that heats up and maximum temperature, further needs exist in number
According to " temperature-resistance " test pattern is selected in logging software, now system is by the temperature on lasting receiving tank vivo sample support
Temperature sensor data, and using temperature as ordinate, resistance value is abscissa record data.If the resistance applied to gas sensitive
Research, then need to select " gas piezo-resistive " test function in data logging software, now system will be gathered and recorded in tank body
The barometric data of numeral, and using air pressure as abscissa, resistance is that ordinate is recorded.Extra dispensing source of the gas is needed to being applied in tank
Plus-pressure, so as to meet the environmental requirement of sample resistance measurement.
When using inflammable and explosive hazardous gas, if leak, or when monitoring that pressure inside the tank exceedes alarm level, it is close
The automatic pressure-controlled valve installed in capping will start vacuum pumping, can also manually boot vacuum pumping, to avoid the occurrence of safety
Problem.
After the completion of resistance measurement, data result output form is selected first in the data logging software of host computer, can be set
It is set to Excel Output of for ms, or the output of Txt text documents form.
The power supply of multichannel resistance measuring instrument is closed, hermetically sealed can is vacuumized or the operation that cools, treats that temperature reaches
After end being vacuumized in room temperature or tank, you can open closure, remove the fixed probe of high flux four, release specimen holder
It is fixed, take out sample and terminate to test.
Embodiment 1
The present embodiment is so that using high throughput method, screening one kind has minimum resistance temperature effect from certain ternary material
Composition exemplified by, to illustrate the research application of high flux In-situ resistance test equipment.The present embodiment comprises the following steps that：
A1, choose what is prepared using combined chip method, using 3 inches of quartz plates as substrate, surface is coated with 64 independently of each other
And the different size of composition is A × A (A=1~3mm) certain ternary material film sample.Sample pallet is put into, is adjusted
Position and fixation.
B1, the probe of high flux four is fixed using bolt with sample pallet, due to the preparation of sample and setting for probe
Meter employs compatible size, and the probe now popped one's head in can just contact well with sample surfaces correct position.
C1, it will be connected inside the electrical connector of the cable plug of four probes and tank body, cover air sealing cover simultaneously
Fixed with bolt, complete the airtight test to tank body and vacuumize, to prevent temperature-rise period from sample oxidation occur, be passed through 2MPa
Argon gas is as protective gas.Then with client cables by outside tank body electrical connector with the probe instrument of multichannel four
Input/output terminal connects.
D1, the data logging software of host computer is opened, constant-current source and voltage collection circuit configuration are set to give tacit consent to, and select instrument
" temperature-resistance " measurement pattern, do not choose " the record time is the second abscissa ", it is 1 DEG C to set thermograph step-length, i.e. temperature
Degree often raises the resistance data for once recording once each sample.
E1, the device parameter of configuration control sample pallet internal resistance heated for controlling temperature original paper, it is 25 DEG C to set initial temperature,
Heating mode is arranged to step-by-step movement, i.e. temperature often raises 1 DEG C and is then incubated 3s, is then further continued for heating up, and heating maximum temperature is 200
℃。
F1, host computer data logging software record start button is clicked on, open heating device control power supply, system will be automatic
64 samples are recorded from 25~200 DEG C, with 1 DEG C of resistance data for step-length.
G1, after test terminates, heating controller is closed, it is Excel to select the data output form in data logging software
Output, chooses data storage catalogue and preserves.
H1, after waiting sample temperature to be cooled to room temperature, manually opened vavuum pump, intraductal atmospheric pressure is evacuated to 1bar or so, opened
Air sealing cover, four probes are dismantled, take out Sample storage, closed the power supply being connected with equipment, put cable in order.
I1, using data in Excel, using temperature as abscissa, the resistance of each sample is respectively ordinate, soft mapping
Drawn in part and there emerged a the curve that sample resistance varies with temperature, therefrom selected resistance and vary with temperature the minimum sample of slope correspondingly
Composition, in as this ternary material, the minimum target component of temperature-coefficient of electrical resistance.
Embodiment 2
The present embodiment is so that using high throughput method, screening one kind has the most fast quick resistance of hydrogen from certain ternary hydrogen quick material
Exemplified by the composition of response, to illustrate the research application of high flux In-situ resistance test equipment.The present embodiment comprises the following steps that：
A2, choose what is prepared using combined chip method, using 3 inches of quartz plates as substrate, surface is coated with 64 independently of each other
And the different size of composition is B × B (A=1~3mm) certain ternary material film sample.Sample pallet is put into, is adjusted
Position and fixation.
B2, the probe of high flux four is fixed using bolt with sample pallet, due to the preparation of sample and setting for probe
Meter employs compatible size, and the probe now popped one's head in can just contact well with sample surfaces correct position.
C2, it will be connected inside the electrical connector of the cable plug of four probes and tank body, cover closure and be used in combination
Bolt is fixed, and is completed the airtight test to tank body and is vacuumized.Then with client cables by outside tank body electrical connector with
The input/output terminal of the probe instrument of multichannel four connects.
D2, the data logging software of host computer is opened, constant-current source and voltage collection circuit configuration are set to give tacit consent to, and select instrument
" gas piezo-resistive " measurement pattern, choose " the record time is the second abscissa ", set resistance time record step-length be
0.1s, i.e., each sample, at interval of 0.1 second record, one resistance value.
E2, the device parameter of configuration control sample pallet internal resistance heated for controlling temperature original paper, it is 25 DEG C to set initial temperature,
Heating rate is 5 DEG C/min, and target temperature is 60 DEG C, soaking time 100h.Heating heating power supply is opened, waits sample temperature
Reach 60 DEG C and stably.
F2, host computer data logging software record start button is clicked on, setting hydrogen cylinder pressure-reducing valve low-pressure side air pressure is
0.1MPa, intake valve is opened, rapidly to 0.1MPa H2 are passed through in tight tank, now software will record air pressure change in tank, with
And each sample resistance changes with time after being passed through H2, i.e. the quick electrical response of hydrogen of sample.Wait 30min.Open vavuum pump
And vacuum valve, the H2 in tank is extracted within 3s, then 0.1MPa argon gas is passed through in very short time, now software records is
After removing H2 atmosphere, the response characteristic of each sample resistance.30min is waited, argon gas is extracted again, is passed through 0.1MPa hydrogen afterwards
Gas, electrical response characteristic of each sample to hydrogen in now second of cyclic process of sample record.So 10 times repeatedly.
G2, after test terminates, atmosphere in tank is extracted first, then passes to 0.1MPa argon gas.Close heating controller, choosing
The data output form selected in data logging software exports for Excel, chooses data storage catalogue and preserves.
H2, after waiting sample temperature to be cooled to room temperature, manually opened vavuum pump, intraductal atmospheric pressure is evacuated to 1bar or so, opened
Air sealing cover, four probes are dismantled, take out Sample storage, closed the power supply being connected with equipment, put cable in order.
I2, using data in Excel, using temperature as abscissa, the resistance of each sample is respectively ordinate, soft mapping
In part draw there emerged a the curve that sample resistance varies with temperature, therefrom can be according to hydrogen and removal hydrogen be passed through after, each sample
Resistance change with time speed screening remove this ternary material in have the quick electrical response characteristic of most quick hydrogen composition, separately
Outside, according to circulation 10 times after each sample the quick electrical response speed of hydrogen, judgement there is property retention best in cyclic process
The material composition of rate.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (8)
- A kind of 1. probe in-situ resistivity-measuring devices of high flux material chip four, it is characterised in that：Visited including the probe of high flux four Head (1), the airtight tank body of high temperature high voltage resistant (2), sample pallet (3), the probe instrument of multichannel four (6), transmission cable (5) With data logging software (7)；Sample pallet (3) is located in the airtight tank body of high temperature high voltage resistant (2), the probe of high flux four (1) On sample pallet (3), the probe of high flux four (1) is surveyed by the probe resistance of transmission cable (5) connecting multi-channel four Instrument (6) is tried, data logging software (7) is installed on host computer, and data logging software (7) receives to be surveyed from the probe resistance of multichannel four The data of instrument (6) measurement are tried, and carry out real-time display and record.
- 2. the probe in-situ resistivity-measuring devices of high flux material chip four according to claim 1, it is characterised in that：It is described The airtight tank body of high temperature high voltage resistant (2) is used to provide the pressure and atmosphere needed for reaction, by top cover labyrinth (4) to high temperature high voltage resistant Airtight tank body (2) is sealed；The airtight tank body of high temperature high voltage resistant (2) uses high-class stainless steel material, internally no more than 500 DEG C Used with conditions of 6MPa pressure, noncorrosive gases reacts in the airtight tank body of high temperature high voltage resistant (2) with sample.
- 3. the probe in-situ resistivity-measuring devices of high flux material chip four according to claim 2, it is characterised in that：It is described The airtight tank body of high temperature high voltage resistant (2) is provided with electric coupler part, for the high flux four in the airtight tank body of high temperature high voltage resistant (2) The cable of the cable of probe and the outside probe instrument of multichannel four is attached；Top cover labyrinth (4) is provided with gas Pressure and temperature instrument, and over-pressure over-temperature alarm assemblies and relief valve are provided with, it is additionally provided with urgent exhaust passage, emergency exhausting pipe Road can empty the gas in the airtight tank body of high temperature high voltage resistant (2) within 1~3s.
- 4. the probe in-situ resistivity-measuring devices of high flux material chip four according to claim 1, it is characterised in that：It is described The probe of high flux four (1) includes shell (11), fixed knob (12), cable jointing (13) and probe (14), high pass Measure four probes (1) be used for install the probe (14) that is directly contacted with sample, buffer unit built in probe (14) can be with sample The non-rigid contact in product surface, probe (14) spacing are fixed；Cable jointing (13) is located in shell (11), fixed knob (12) It is fixed for the probe of high flux four (1) and sample pallet (3).
- 5. the probe in-situ resistivity-measuring devices of high flux material chip four according to claim 1, it is characterised in that：It is described Transmission cable (5) inner lead is high temperature resistant material, and all using twisted-pair feeder shielding processing.
- 6. the probe in-situ resistivity-measuring devices of high flux material chip four according to claim 1, it is characterised in that：It is described Sample pallet (3) uses monolithic construction, and resistance heating device and Temperature-controlled appliance are provided with inside sample pallet (3), by The outside Switching Power Supply power supply of the airtight tank body of high temperature high voltage resistant (2)；Sample pallet (3) includes interface (31), knob (32), pedestal (33) it is located at fixture (34), interface (31), knob (32) and fixture (34) on pedestal (33), interface (31) is used for and high flux Four probes (1) connect, and knob (32) is used to adjust sample position, and fixture (34) is used to adjusting and fixing sample position.
- 7. the probe in-situ resistivity-measuring devices of high flux material chip four according to claim 1, it is characterised in that：It is described The probe instrument of multichannel four (6) uses integral structure, has been internally integrated in a shell structure including 64 passages The voltage-controlled constant-current supply module of high accuracy, microprocessor control module, 64 channel voltages that constant current size can be independently arranged are adopted Sample circuit and high-precision degree type ADC, temperature detecting module, communication module, peripheral interface circuit and switch power module；It is more logical Joint (61), four pin data-interfaces (62), LCD display (63), measurement pattern are set outside the probe instrument of road four (6) Selecting switch (64), LCD brightness regulation knobs (65) and total power switch (66), joint (61) are used to complete number with transmission cable According to input and output, four pin data-interfaces (62) are the binding post of 1~8 passage, and the sample frequency of each passage is remembered in data Set in recording software (7), highest sample frequency is more than 50 times/second.
- 8. the probe in-situ resistivity-measuring devices of high flux material chip four according to claim 1, it is characterised in that：It is described Current resistive value that data logging software (7) real-time display measures and resistance value with the time, air pressure, temperature change curve, will Data are exported in the form of Excel or txt text document files.
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