CN109974896A - A kind of miniature calibration source chip of water triple point - Google Patents
A kind of miniature calibration source chip of water triple point Download PDFInfo
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- CN109974896A CN109974896A CN201910235278.XA CN201910235278A CN109974896A CN 109974896 A CN109974896 A CN 109974896A CN 201910235278 A CN201910235278 A CN 201910235278A CN 109974896 A CN109974896 A CN 109974896A
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- water
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- triple point
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- calibration source
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K15/00—Testing or calibrating of thermometers
- G01K15/005—Calibration
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Abstract
The invention belongs to semiconductor material and its fabricating technology fields, it is related to a kind of miniature calibration source chip of water triple point, its main structure includes silica shell, vacuum interlayer, water body and Three Dimensional Cavities, Three Dimensional Cavities are constituted in the intracavity space of the chamber shape silica shell of three-dimensional structure, the space of Three Dimensional Cavities is divided into up-down structure, water body is constituted filled with pure water in the cavity of lower part, the cavity on top constitutes vacuum interlayer, vacuum interlayer and water body are sealed in Three Dimensional Cavities, and the external of Three Dimensional Cavities constitutes closed silica shell and form chip structure；The chip structure that it is designed is scientific and reasonable, simple process, and extensively, stable and reliable for performance, application field is extensive, and temperature sensitive significant effect, preparation process and equipment are simple for material selection, and technological means is mature, saves the energy, and application environment is friendly.
Description
Technical field:
The invention belongs to semiconductor material and its device preparation technology technical fields, are related to a kind of miniature calibration of water triple point
The structure of source chip designs, and using the bonding techniques between chip, realizes water triple point bottle in the production of micron dimension, in semiconductor
The Wen Ping that water triple point is presented in the Three Dimensional Cavities of the micron scale construction of material, provides the scale of thermometer under microstructure and state
It is fixed.
Background technique:
In the every field of daily life and science and technology, temperature is an important and special fundamental physical quantity, temperature
Degree meterological is an important branch in meterological field；Especially in each of scientific research and industrial and agricultural production ring
Section be unable to do without and the reliable of temperature is accurately measured and its controlled.For a long time, people are for temperature measurements made,
Only position of the temperature on temperature scale makes temperature scale occupy extremely important status in temperature measurement, and temperature scale is temperature
Accurately, the basis of reliable measurements, in a country, the foundation of temperature scale and the metering for implementing to reflect this country from a side
The height of scientific and technological level and technical standard.
In numerous materials, the triple point of water is not only the unique reference point and ITS- of thermodynamic temperature
The most important fixed point that 90 international temperature scales define, it is surveyed in thermodynamic temperature measurement, international temperature scale reproduction and actual temperature
In amount, all have a very important significance.Therefore, water triple point correctly reappears and accurate measurement is that ITS-90 international temperature scale is implemented
Key.
With the development of the wafer bonding techniques of semiconductor material, application is more and more extensive, wafer bonding techniques
Basic principle is to make the chip realization of the identical or different material preparation of two panels long-term steady by the methods of physics, chemistry and machinery
Fixed combination, the technology can produce artificial synthesized new material and be used to manufacture new structural semiconductor material devices, very
It can extremely be used to manufacture more complex three-dimensional structure chip；And Miniature water three is made using wafer bonding techniques in the prior art
The technology of the miniature calibration chip of phase point there is not yet mature embodiment disclosure.
Currently, water triple point is the jelly system by water triple point bottle and saves to reappear, traditional water triple point bottle knot
Structure size is larger, during reproduction, needs the processes such as pre-cooling, freezing ice sleeve, required time is longer.Therefore, one kind was researched and developed both
It can be drawn out to the miniature calibration source chip of water triple point that outer wall measures in intracavitary thermometric or by temperature, realize and be based on water three
The warm level ground of phase point carry out temperature correction device be it is very necessary, this is for the in situ online real-time of the following internet of things sensors
Calibration is of great significance；It avoids sensor and needs to be sent back to the cumbersome process that laboratory is calibrated, it is especially corresponding
In-situ monitoring under deep-sea, space, remote and adverse circumstances is significant.
Summary of the invention:
It is an object of the invention to overcome it is of the existing technology can not real time calibration in situ the shortcomings that, utilize bonding chip
Technology design constructs a kind of miniature calibration source chip of water triple point and subtracts for realizing the real time calibration in situ to temperature sensor
The volume of small water triple point bottle；Its chip structure is to the fields such as physics, biological and chemical sensitisation, hydrospace detection and space technology
Development has important practical value and scientific meaning.
To achieve the goals above, the main structure of the miniature calibration source chip of water triple point of the present invention includes dioxy
SiClx shell, vacuum interlayer, water body and Three Dimensional Cavities are constituted in the intracavity space of the chamber shape silica shell of three-dimensional structure
Three Dimensional Cavities, the space of Three Dimensional Cavities are divided into up-down structure, constitute water body, the cavity on top filled with pure water in the cavity of lower part
Vacuum interlayer is constituted, vacuum interlayer and water body are sealed in Three Dimensional Cavities, and the external of Three Dimensional Cavities constitutes closed silica
Shell simultaneously forms chip structure；Gas phase, liquid phase and solid phase of the water body when temperature is 0.01 DEG C and pressure is 4.58mmHg coexist, and three
When mutually coexisting the temperature of water body can be maintained in 1 millisecond to 2 hours 0.01 DEG C it is constant and form Wen Ping；The purity of water body is not
It does not include metallic ingredient in impurity contained therein less than 99.99%；The space or volume ratio of vacuum insulation layer and water body are 1:
0.5--5 calibrates the structure size of source chip at several centimeters to nanometer scale；The raw material of calibration source chip include quartz, partly lead
Body material, crystalline material, high-molecular compound material, metal material, plastics, PDMS (dimethyl silicone polymer), PMMA (poly- first
Base methyl acrylate) or COC (cyclic olefin polymer)；Wherein semiconductor material includes the arsenic of the silicon of IV race, III-V compound
Change gallium, indium phosphide or II-VI group compound；When the preparation of the related miniature calibration source chip of water triple point, first by two two
Silica or quartz wafer or growth have the silica-base material substrate of silicon dioxide layer thoroughly to be cleaned, then in first base
On piece etches a three-dimensional cavity structure；Two substrates are placed in a confined space after clean the surface again and extract air
610.75 pa of vacuum degree is formed, formula is fixed using bonding method after being then directed at second substrate with first substrate and is glued
It closes, then pressure and temperature is applied to two substrates and realizes the pre- bonding of two substrates, then carry out the high temperature anneal completion
The complete bonding of two substrates；Chip cutting and reduction processing are finally carried out again, obtain the miniature calibration source chip of water triple point.
The volume of the Three Dimensional Cavities of the three-dimensional cavity-like structure of the miniature calibration source chip of water triple point of the present invention is from 10
Cubic nanometer is to 500 cubic centimetres；The inner-wall material of Three Dimensional Cavities include silica or silicon (including monocrystalline silicon, polysilicon,
Amorphous silicon) or quartz crystal slice etch；Fluid channel is etched in silicon dioxide layer and is connected with Three Dimensional Cavities, then by pre- key
Two substrates after conjunction, which are put into annealing furnace, to be made annealing treatment；Substrate after annealing is thinned and is sliced, water three is obtained
The miniature calibration source chip of phase point；Fluid channel is connect with water syringe and minipump, pure water, shape are injected into Three Dimensional Cavities
Inside cavity pressure at water body part is water triple point pressure values 610.75Pa；It is close by being realized to miniflow road junction heating melting
Seal miniflow road junction.
The miniature calibration source chip of water triple point of the present invention includes at least one Three Dimensional Cavities, the inner wall of Three Dimensional Cavities
Material includes but is not limited to quartz, III-V material, such as GaAs and indium phosphide or macromolecule polymer material, such as
COC (cyclic olefin polymer), PDMS (dimethyl silicone polymer), PMMA (polymethyl methacrylate) or plastic material or gold
Belong to material or II-VI group material or IV race material silicon.
The Three Dimensional Cavities of solid cavity-like structure of the present invention are etched by silicon crystal piece；Or the three-dimensional chamber
Body is etched by iii-v crystal wafer；Or the Three Dimensional Cavities are etched by II-VI group crystal wafer；Or it is described
Three Dimensional Cavities be to be etched by IV group crystal piece；Or the Three Dimensional Cavities be by macromolecule polymer material etching and
At；Or the Three Dimensional Cavities are etched by quartz material；Or the Three Dimensional Cavities are imprinted by plastic material.
Bonding between two substrates of the present invention is by being bonded growth metallic film on section in substrate and heating
Metal is allowed to gapless bonding；Or by chemical method, adhesive is smeared in substrate interface and is allowed to gapless bonding.
Compared with prior art, the present invention the chip structure of its design is scientific and reasonable, simple process, material selection is extensive,
Stable and reliable for performance, application field is extensive, and temperature sensitive significant effect, preparation process and equipment are simple, and technological means is mature, saves energy
Source, application environment are friendly.
Detailed description of the invention:
Fig. 1 is the miniature calibration source chip body principle schematic diagram of water triple point of the invention.
Fig. 2 is the miniature calibration source chip preparing process schematic process flow diagram of water triple point of the invention.
Fig. 3 is the technical process schematic diagram of the specific embodiment of the miniature calibration source chip preparation of water triple point of the invention.
Fig. 4 is the technical process schematic diagram that the miniature calibration source chip of water triple point of the invention prepares another embodiment.
Fig. 5 is the warm plateau curve figure of the miniature calibration source chip of water triple point of the invention.
Specific embodiment:
The present invention is described further by way of example and in conjunction with the accompanying drawings.
Embodiment 1:
The main structure of the miniature calibration source chip of the water triple point that the present embodiment is related to include silica shell 1, vacuum every
Layer 2, water body 3 and Three Dimensional Cavities 4, constitute Three Dimensional Cavities in the intracavity space of the rectangular silica shell 1 of three-dimensional structure
4, the space of Three Dimensional Cavities 4 is divided into up-down structure, constitutes water body 3 filled with pure water in the cavity of lower part, and the cavity on top is constituted
Vacuum interlayer 2, vacuum interlayer 2 and water body 3 are sealed in Three Dimensional Cavities 4, and the external of cavity 4 constitutes closed silica shell 1
And form chip structure；Water body 3 gas phase, liquid phase and solid phase when temperature is 0.01 DEG C and pressure is 4.58mmHg coexist, at this time
The temperature of water body 3 can be maintained in 1 millisecond to 2 hours 0.01 DEG C it is constant and form Wen Ping, as shown in Figure 5；Water body 3 uses
The purity of pure water is not less than 99.99%, does not include metallic ingredient in impurity contained therein；Vacuum insulation layer 2 and water body 3
Space or volume ratio are 1:0.5--5.
The preparation process of the miniature calibration source chip of the water triple point that the present embodiment is related to include etching silicon dioxide shell,
Etching fluid channel, cleaning substrate, substrate bonding, high annealing, thinned charge with slice, water body seal with fluid channel, specific
Processing step are as follows:
(1) etching silicon dioxide shell: choosing the substrate that two panels surface is silicon dioxide layer, and substrate is quartz wafer or growth
There is the silicon wafer of silica；The silicon dioxide layer of one of substrate is etched into the rectangular depression being sized, completes dioxy
It is prepared by the part of SiClx shell 1；
(2) it etches fluid channel: going out micro flow channel slot in the surface etch of a substrate；The etching and rectangular depression of fluid channel
Lithographic method it is similar, after first passing through surface treatment, smear photoresist, then carry out optical exposure and development technique obtain needed for
Photoetching offset plate figure, photoetching offset plate figure is then transferred to by material surface by lithographic technique (such as wet etching, dry etching),
The size of fluid channel is set according to the size of chip；
(3) it cleans substrate: two substrates is cleaned, remove surface contamination, guarantee that substrate surface is clean, smooth and light
It is clean, meet bonding conditions；
(4) substrate is bonded in advance: two closed bondings of substrate merging one are intracavitary, and bonding chamber is connected to vacuum pump, vacuumizes
To the pressure of 4.58mmHg；Second substrate is aligned with the substrate for being etched with rectangular recess and is set to be put into heating
Then the room temperature being heated under vacuum between two metal plates of function applies 0.1- to two panels metal plate to 500 DEG C of temperature
0.2MPa pressure closes silica shell 1 using direct key is legal, makes to form sealed environment inside its rectangular depression, constitute
Three Dimensional Cavities；
(5) silica shell 1 for the silica chip architecture being in vacuo bonded high annealing: is sent into annealing furnace
In, it is to be made annealing treatment in 800-1100 DEG C of environment in temperature, annealing time was less than 2 hours；
(6) it is thinned with slice: the titanium dioxide silicon wafer being bonded being thinned, slicing treatment respectively, obtain water three
Then the miniature calibration source chip of phase point connects micro-channel again for runner；
(7) water body charges: pure water is instilled by micro-channel in the Three Dimensional Cavities 4 of the rectangular recess structure of etching,
Water in Three Dimensional Cavities 4 is without filling, and keeping the gas pressure intensity in Three Dimensional Cavities 4 is 4.58mmHg；
(8) fluid channel seals: by heating so that sealing is realized in the melting of miniflow road junction；Micro-channel is by fluid channel and extraneous
It is connected, the material of micro-channel is thermoplastic resin material, and fusing point is lower than 100 DEG C, is melted using electric iron to pipeline
Sealing, electric iron is powered, and temperature reaches preset temperature (being higher than tubing fusing point), by electric iron slowly close to tubing, makes tubing
Melting, so that fluid channel is isolated from the outside world；Complete the miniature calibration source chip product of water triple point.
The method of the bonding of substrate involved in the step of the present embodiment (4) includes physics, chemistry and mechanical means, passes through control
The technology of pressing pressure, Wen Rong and adhesion process is realized, or the partial region growth metal in the bonding section of two substrates leads to again
It crosses and METAL HEATING PROCESS is bonded；Or the interface being bonded at two carries out closed sticked type bonding by chemical adhesive；It is prepared into
The temperature of the miniature calibration source chip of water triple point, the fields such as the industry being related to for temperature sensor, agricultural and intelligent control is surveyed
Control and calibration.
Embodiment 2:
The main structure of the miniature calibration source chip of the water triple point that the present embodiment is related to include silica shell 1, vacuum every
Layer 2, water body 3 and Three Dimensional Cavities 4 constitute water body 3 in the inside irrigation pure water of the silica shell 1 of three-dimensional structure；Water body 3
Gas phase, liquid phase and solid phase three-phase coexistence when temperature is 0.01 DEG C and pressure is 4.58mmHg, coolant-temperature gage can be in 1 milli at this time
Be maintained in seconds -2 hours time 0.01 DEG C it is constant and form Wen Ping, as shown in Figure 5.
The preparation process of the miniature calibration source chip of the water triple point that the present embodiment is related to is substantially the same manner as Example 1,
Difference is the method for Three Dimensional Cavities with the extraneous fluid channel that is connected, and first carries out to upper substrate before slice thinned, then etches
Cylindrical channel is sliced again after communicating the external world with fluid channel；Concrete operation step refers to attached drawing 4.
The shape of the miniature calibration source chip of water triple point prepared by embodiment 1 and embodiment 2 is rectangular parallelepiped structure, size
In several hundred microns to several millimeter magnitudes；In use, using TEC (semiconductor cooler) by temperature control -8 DEG C to 4 DEG C it
Between, chip is placed in above TEC, and entire chip temperature is first down to -8 DEG C by TEC, and the jelly time processed is short, and then temperature rises to 4 DEG C,
In temperature ramp de the phase transformation of water occurs at 0.01 DEG C for chip, and constant temperature is made to be maintained at 0.01 DEG C, forms a period of time
Wen Ping；Chip temperature has the uncertainty of 0.1mK, is mainly used in physics, biology and chemical sensitisation, hydrospace detection and boat
The fields such as its technology, such as the calibration of platinum resistance chip and thermal resistance chip, effect is superior to many index of the prior art, and
Its temperature scale is stablized, and calibration degree is high.
Claims (4)
1. a kind of miniature calibration source chip of water triple point, main structure includes silica shell, vacuum interlayer, water body and three-dimensional chamber
Body, it is characterised in that constitute Three Dimensional Cavities, Three Dimensional Cavities in the intracavity space of the chamber shape silica shell of three-dimensional structure
Space be divided into up-down structure, constitute water body filled with pure water in the cavity of lower part, the cavity on top constitutes vacuum interlayer, vacuum
Interlayer and water body are sealed in Three Dimensional Cavities, and the external of Three Dimensional Cavities constitutes closed silica shell and form chip structure；
Gas phase, liquid phase and solid phase of the water body when temperature is 0.01 DEG C and pressure is 4.58mmHg coexist, the temperature of water body when three-phase coexistence
Degree can be maintained in 1 millisecond to 2 hours 0.01 DEG C it is constant and form Wen Ping；The purity of water body is not less than 99.99%, wherein
It does not include metallic ingredient in impurities；The space or volume ratio of vacuum insulation layer and water body are 1:0.5--5, calibrate source core
The structure size of piece arrives nanometer scale at several centimeters；The raw material for calibrating source chip include quartz, semiconductor material, crystal material
Material, high-molecular compound material, metal material, plastics, PDMS (dimethyl silicone polymer), PMMA (polymethyl methacrylate)
Or COC (cyclic olefin polymer)；Wherein semiconductor material includes the silicon of IV race, the GaAs of III-V compound, indium phosphide,
Or II-VI group compound；When the preparation of the miniature calibration source chip of water triple point, first by two silica or quartz wafer or
Growth has the silica-base material substrate of silicon dioxide layer thoroughly to be cleaned, and a three-dimensional chamber is then etched on first substrate
Body structure；Two substrates are placed in a confined space after clean the surface again and extract air formation 610.75 pa of vacuum degree,
Formula bonding is fixed using bonding method after then second substrate is aligned with first substrate, then two substrates are applied
Then pressure and temperature and the pre- bonding for realizing two substrates carry out the complete bonding that the high temperature anneal completes two substrates；
Chip cutting and reduction processing are finally carried out again, obtain the miniature calibration source chip of water triple point.
2. the miniature calibration source chip of water triple point according to claim 1, it is characterised in that the miniature calibration source of water triple point
The volume of the Three Dimensional Cavities of the three-dimensional cavity-like structure of chip is from 10 cubic nanometers to 500 cubic centimetres；The inner wall material of Three Dimensional Cavities
Material is by including that silica or silicon or quartz crystal slice etch；Fluid channel is etched in silicon dioxide layer and with three-dimensional chamber
Body connection, then two substrates after pre- bonding are put into annealing furnace and are made annealing treatment；Substrate after annealing is carried out thinned
With slice, the miniature calibration source chip of water triple point is obtained；Fluid channel is connect with water syringe and minipump, Xiang Sanwei chamber
Injection pure water in vivo, the inside cavity pressure for forming water body part is water triple point pressure values 610.75Pa；By to fluid channel
Mouth heating melting realizes sealing miniflow road junction.
3. the miniature calibration source chip of water triple point according to claim 1, it is characterised in that the miniature calibration source of water triple point
Chip includes at least one Three Dimensional Cavities.
4. the miniature calibration source chip of water triple point according to claim 1, it is characterised in that the bonding between two substrates
Gapless bonding is allowed to by being bonded on section to grow metallic film and heat metal in substrate；Or by chemical method, in base
Adhesive is smeared on piece interface is allowed to gapless bonding.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910235278.XA CN109974896B (en) | 2019-03-27 | 2019-03-27 | Water triple point miniature calibration source chip |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910235278.XA CN109974896B (en) | 2019-03-27 | 2019-03-27 | Water triple point miniature calibration source chip |
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| CN109974896A true CN109974896A (en) | 2019-07-05 |
| CN109974896B CN109974896B (en) | 2020-07-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110887584A (en) * | 2019-11-11 | 2020-03-17 | 德州尧鼎光电科技有限公司 | Miniature water triple-point bottle and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MXPA98000752A (en) * | 1998-01-27 | 2003-10-14 | Ct Nac De Metrologia | Double-chamber cell for the water triple point reproduction. |
| KR20050110366A (en) * | 2004-05-18 | 2005-11-23 | 한국표준과학연구원 | Maintenance method and container of triple point of water cell |
| CN203287123U (en) * | 2013-02-01 | 2013-11-13 | 深圳市艾依康仪器仪表科技有限公司 | Device for manufacturing ice mantle in water three-phase point bottle |
| CN109632143A (en) * | 2019-01-22 | 2019-04-16 | 中国计量科学研究院 | A kind of self calibration clinical thermometer |
-
2019
- 2019-03-27 CN CN201910235278.XA patent/CN109974896B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MXPA98000752A (en) * | 1998-01-27 | 2003-10-14 | Ct Nac De Metrologia | Double-chamber cell for the water triple point reproduction. |
| KR20050110366A (en) * | 2004-05-18 | 2005-11-23 | 한국표준과학연구원 | Maintenance method and container of triple point of water cell |
| CN203287123U (en) * | 2013-02-01 | 2013-11-13 | 深圳市艾依康仪器仪表科技有限公司 | Device for manufacturing ice mantle in water three-phase point bottle |
| CN109632143A (en) * | 2019-01-22 | 2019-04-16 | 中国计量科学研究院 | A kind of self calibration clinical thermometer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110887584A (en) * | 2019-11-11 | 2020-03-17 | 德州尧鼎光电科技有限公司 | Miniature water triple-point bottle and manufacturing method thereof |
| CN110887584B (en) * | 2019-11-11 | 2022-05-10 | 德州尧鼎光电科技有限公司 | Miniature water triple-point bottle and manufacturing method thereof |
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