CN102522490A - Preparation method for glass micro-needle thermocouple - Google Patents
Preparation method for glass micro-needle thermocouple Download PDFInfo
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- CN102522490A CN102522490A CN2011103720443A CN201110372044A CN102522490A CN 102522490 A CN102522490 A CN 102522490A CN 2011103720443 A CN2011103720443 A CN 2011103720443A CN 201110372044 A CN201110372044 A CN 201110372044A CN 102522490 A CN102522490 A CN 102522490A
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- 239000011521 glass Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
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- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- 238000000151 deposition Methods 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000005336 cracking Methods 0.000 claims abstract description 7
- 229920006254 polymer film Polymers 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 39
- 230000008021 deposition Effects 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
- 239000010409 thin film Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011160 research Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
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- VRBFTYUMFJWSJY-UHFFFAOYSA-N 28804-46-8 Chemical compound ClC1CC(C=C2)=CC=C2C(Cl)CC2=CC=C1C=C2 VRBFTYUMFJWSJY-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 229910000861 Mg alloy Inorganic materials 0.000 description 4
- PGTXKIZLOWULDJ-UHFFFAOYSA-N [Mg].[Zn] Chemical compound [Mg].[Zn] PGTXKIZLOWULDJ-UHFFFAOYSA-N 0.000 description 4
- 229910000679 solder Inorganic materials 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
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- 206010028980 Neoplasm Diseases 0.000 description 1
- 208000024799 Thyroid disease Diseases 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 208000010396 acute flaccid myelitis Diseases 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
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- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
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- 230000002588 toxic effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The invention discloses a preparation method for a glass micro-needle thermocouple in the field of biomedical engineering. The preparation method comprises the steps of: depositing a polymer film on the surface of a glass micro-needle; putting the glass micro-needle in a high-temperature environment for cracking to generate a carbon film on the glass micro-needle; filling metal liquid in the glass micro-needle and cooling; grinding the tip of the glass micro-needle to obtain a certain angle; and finally depositing a metal film at the tip of the glass micro-needle to form a thermocouple end junction point to obtain the required glass micro-needle thermocouple. The preparation method has the advantages that the process for preparing the glass micro-needle thermocouple is simple and easy to operate; by adopting the carbon film and biocompatible metal as thermocouple materials, the thermoelectric property is stable, the physical and chemical stability is enough and the thermocouple is not apt to be oxidized or corroded; the temperature coefficient of resistance is small, the conductivity is high and the specific heat is small; the material reproducibility is good and the mechanical strength is high; and the biocompatibility is high and the thermocouple can be directly used in the biomedical field.
Description
Technical field
The present invention relates to a kind of glass micropipette thermocouple preparation of biomedical engineering field, specifically is a kind of with the preparation method of the surperficial carbon film of inner metal of glass micropipette and micropin as the glass micropipette thermocouple of conductor.
Background technology
See the high speed development in field at micro-nano along with biotechnology, semiconductor technology etc.; Research to micro-scaled structures and material receives increasing concern; Especially in the experimental technique field; Can carry out the focus that direct, real-time detection and manipulation become the minute yardstick research field at the detected object of micro/nano-scale to characteristic dimension, also be the challenging research topic that researchers face.Along with the development of AFM, ESEM, ultrafast light source, making the research of calorifics, machinery, chemistry, electricity, optics and acoustical behavior of material detect becomes possibility.
The minute yardstick detection technique plays a part very important in biological activity and other a lot of physical process researchs.For example, the temperature detection of individual cells can provide important data in the thermotropic denaturalization of activity, thyroid disease diagnosis, nucleic acid and the protein of heat therapy, cancer detection, metabolin.The real-time detection of individual cells temperature is a popular research field, and the thermal response of research individual cells in bioprocess can provide important physical information.
Thermocouple can directly be measured temperature, and converts temperature signal to the thermo-electromotive force signal, converts the temperature of measured medium to through electric meter.The basic principle of thermocouple temperature measurement is that conductor (being called thermocouple wire material or the thermode) two ends of two kinds of different components are bonded into the loop; When the temperature at two junction points not simultaneously; In the loop, will produce electromotive force, this phenomenon is called thermoelectric effect, and this electromotive force is called thermoelectric potential.Wherein, directly the end as the measuring media temperature is called working end (being also referred to as measuring junction), and the other end is called cold junction (being also referred to as the compensation end), and cold junction is connected with Displaying Meter or matching instrument, and Displaying Meter can be pointed out the thermoelectric potential that thermocouple produces.In the actual thermometric of thermocouple is used, often adopt the form of hot junction welding, cold junction open circuit, cold junction connects and composes temp measuring system through connecting lead and Displaying Meter.
Theoretically, any two kinds of different conductors (or semiconductor) can be mixed with thermocouple, but as practical temperature element, are many-sided to its requirement.In order to guarantee the reliability in the engineering, and enough certainties of measurement, not all material can both be formed thermocouple; General electrode material to thermocouple; Basic demand is: (1), in temperature-measuring range, and thermoelectric property is stable, not time to time change; Enough physical and chemical stabilities are arranged, be difficult for oxidation or corrosion; (2), temperature coefficient of resistance is little, conductance is high, specific heat is little; (3), produce thermoelectric potential in the thermometric and want big, and be linear between thermoelectric potential and the temperature or near linear monotropic function relation; (4), the material replicability is good, mechanical strength is high, manufacturing process is simple, low price.
Retrieval through to the prior art document is found; R.Shrestha; T.Y.Choi, W.S.Chang etc. write articles " Micropipette-Based Thermal Sensor for Biological Applications " (" based on the biotemperature transducer of micropin " " IEEE transducer in 2010 meeting ") at " IEEE SENSORS 2010 Conference " (2010) p422-445.The nickel that adopts inner tin that feeds of glass micropipette and glass micropipette surface deposition in this article is as thermocouple material.Therefore the thermocouple probe that this method is made is restricted on using owing to used the metallic nickel of the toxic effect of pair cell.
Summary of the invention
The objective of the invention is to overcome the deficiency and the defective of prior art, propose a kind of preparation method of glass micropipette thermocouple, make the glass micropipette thermocouple can be applied to the temperature survey in biomedical minute yardstick field.Owing to adopt biocompatibility metal and carbon film as thermocouple material, therefore can directly apply to the temperature of measuring individual cells.
The present invention realizes through following technical scheme; The present invention is deposition one layer of polymeric film on glass micropipette at first, secondly glass micropipette is put into the hot environment cracking, on glass micropipette, generates one deck carbon film; In glass micropipette, inject metal liquid and cooling then; Then the glass micropipette tip is ground out certain angle, in the most advanced and sophisticated deposition of glass micropipette layer of metal, obtain final needed glass micropipette thermocouple at last.
The present invention includes following steps:
The first step, at glass micropipette surface deposition one layer of polymeric film.
Described glass micropipette is the quartz glass micropin.
Described glass micropipette tip size is that micron is to nanoscale.
Described deposition is chemical vapour deposition (CVD).
Described polymer thin film thickness is that micron is to nanoscale.
Second step, glass micropipette is put into the hot environment cracking, on glass micropipette, generate one deck carbon film.
Described Pintsch process is meant put into the pyrolysis furnace that is full of protective atmosphere with thin polymer film, with 150～1400 ℃ of temperature heating 0.5～6 hour.
The 3rd step, inject metal liquid in the glass micropipette and cool off.
Described metal liquid is low melting point biocompatibility metal and alloy thereof.
The 4th the step, the glass micropipette tip is ground out angle.
Described grinding under the card grinding appearance, the glass micropipette tip being ground out required angle.
The 5th step, the most advanced and sophisticated deposition of glass micropipette layer of metal film form the pyrometer fire-end junction point, obtain final needed glass micropipette thermocouple.
Described metal is a biocompatibility metal, and thickness is that micron is to nanoscale.
Compared with prior art, it is simple to operation that the present invention prepares glass micropipette thermocouple technical process.Adopt carbon film and biocompatibility metal as thermocouple material, thermoelectric property is stable, and enough physical and chemical stabilities are arranged, and is difficult for oxidation or corrosion; Temperature coefficient of resistance is little, and conductance is high, and specific heat is little; The material replicability is good, and mechanical strength is high; Good biocompatibility can directly apply to biomedical sector.
Description of drawings
Fig. 1 is the embodiment of the invention 1 an implementation process sketch map.
Fig. 2 is the embodiment of the invention 2 implementation process sketch mapes.
Fig. 3 is the embodiment of the invention 3 implementation process sketch mapes.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is that prerequisite is implemented with technical scheme of the present invention, provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
As shown in Figure 1, present embodiment prepares through following steps:
The first step, be 5 microns Parylene C (poly) film at glass micropipette surface chemistry vapour deposition one layer thickness of 0.5 micron of most advanced and sophisticated external diameter, shown in Fig. 1 a, the 1st, Parylene C film, the 2nd, quartz glass micropin.
Second the step, have the glass micropipette of Parylene C film to put into the pyrolysis furnace that is full of nitrogen protection atmosphere surface deposition; With 900 ℃ of temperature heating 1 hour (this operates in 150～1400 ℃ of temperature heating and all can implement in the scope in 0.5～6 hour); Cracking Parylene C film generates one deck carbon film, shown in Fig. 1 b on glass micropipette; 1 is the carbon film, and 2 is the quartz glass micropin.
The 3rd step, inject Pb-free solder liquid in the glass micropipette and cool off, shown in Fig. 1 c, the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, Pb-free solder.
The 4th step, use card grinding appearance grind out 45 ° with the glass micropipette tip, shown in Fig. 1 d, and the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, Pb-free solder.
The gold thin film of the 5th step, the most advanced and sophisticated deposition of glass micropipette one deck 200 nanometer thickness forms the pyrometer fire-end junction point, obtains final needed glass micropipette thermocouple, shown in Fig. 1 e, and the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, Pb-free solder, the 4th, gold thin film.
As shown in Figure 2, present embodiment prepares through following steps:
The first step, be 8 microns PP (polypropylene) film at glass micropipette surface chemistry vapour deposition one layer thickness of 1 micron of most advanced and sophisticated external diameter, shown in Fig. 2 a, the 1st, PP film, the 2nd, quartz glass micropin.
Second step, there is the glass micropipette of PP film to put into the pyrolysis furnace that is full of nitrogen protection atmosphere surface deposition, with 700 ℃ of temperature heating 1 hour, cracking PP film; On glass micropipette, generate one deck carbon film; Shown in Fig. 2 b, 1 is the carbon film, and 2 is the quartz glass micropin.
The 3rd step, in protective atmosphere, inject zinc magnesium alloy liquid in the glass micropipette and cool off, shown in Fig. 2 c, the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, zinc magnesium alloy.
The 4th step, use card grinding appearance grind out 45 ° with the glass micropipette tip, shown in Fig. 2 d, and the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, zinc magnesium alloy.
The gold thin film of the 5th step, the most advanced and sophisticated deposition of glass micropipette one deck 150 nanometer thickness forms the pyrometer fire-end junction point, obtains final needed glass micropipette thermocouple, shown in Fig. 2 e, and the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, zinc magnesium alloy, the 4th, gold thin film.
As shown in Figure 3, present embodiment prepares through following steps:
The first step, be 8 microns GDP (glow discharge polymer) film at glass micropipette surface chemistry vapour deposition one layer thickness of 1 micron of most advanced and sophisticated external diameter, shown in Fig. 3 a, the 1st, GDP film, the 2nd, quartz glass micropin.
Second step, there is the glass micropipette of GDP film to put into the pyrolysis furnace that is full of nitrogen protection atmosphere surface deposition, with 500 ℃ of temperature heating 1 hour, cracking GDP film; On glass micropipette, generate one deck carbon film; Shown in Fig. 3 b, 1 is the carbon film, and 2 is the quartz glass micropin.
The 3rd step, in protective atmosphere, inject the magnesium metal liquid in the glass micropipette and cool off, shown in Fig. 3 c, the 1st, carbon film, the 2nd, magnesium, the 3rd, glass micropipette.
The 4th step, use card grinding appearance grind out 30 ° with the glass micropipette tip, shown in Fig. 3 d, and the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, magnesium metal.
The gold thin film of the 5th step, the most advanced and sophisticated deposition of glass micropipette one deck 200 nanometer thickness forms the pyrometer fire-end junction point, shown in Fig. 3 e, and the 1st, carbon film, the 2nd, quartz glass micropin, the 3rd, magnesium metal, the 4th, gold thin film.
The technology of the foregoing description is simple, easy to operate.Adopt carbon film and biocompatibility metal as thermocouple material, thermoelectric property is stable, and enough physical and chemical stabilities are arranged, and is difficult for oxidation or corrosion; Temperature coefficient of resistance is little, and conductance is high, and specific heat is little; The material replicability is good, and mechanical strength is high; Good biocompatibility can directly apply to biomedical sector.Should be understood that the foregoing description is preferred enforcement of the present invention, the present invention can also be other execution mode, like conversion parameter (like 150～1400 ℃ of Pintsch process temperature, parameters such as angle and time) wherein.
Although content of the present invention has been done detailed introduction through above-mentioned preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (9)
1. the preparation method of a glass micropipette thermocouple is characterized in that may further comprise the steps:
The first step, at glass micropipette surface deposition one layer of polymeric film;
Second step, glass micropipette is put into the hot environment cracking, on glass micropipette, generate one deck carbon film;
The 3rd step, inject metal liquid in the glass micropipette and cool off;
The 4th the step, the glass micropipette tip is ground out angle;
The 5th step, the most advanced and sophisticated deposition of glass micropipette layer of metal film form the pyrometer fire-end junction point, obtain final needed glass micropipette thermocouple.
2. the preparation method of glass micropipette thermocouple according to claim 1 is characterized in that, described glass micropipette is the quartz glass micropin.
3. the preparation method of glass micropipette thermocouple according to claim 1 and 2 is characterized in that, described glass micropipette tip size is that micron is to nanoscale.
4. the preparation method of glass micropipette thermocouple according to claim 1 is characterized in that, described deposition is chemical vapour deposition (CVD).
5. the preparation method of glass micropipette thermocouple according to claim 1 is characterized in that, described Pintsch process is meant puts into the pyrolysis furnace that is full of protective atmosphere with thin polymer film, with 150～1400 ℃ of temperature heating 0.5～6 hour.
6. according to the preparation method of claim 1 or 5 described glass micropipette thermocouples, it is characterized in that described polymer thin film thickness is that micron is to nanoscale.
7. the preparation method of glass micropipette thermocouple according to claim 1 is characterized in that, described metal liquid is low melting point biocompatibility metal and alloy thereof.
8. the preparation method of glass micropipette thermocouple according to claim 1 is characterized in that, described grinding is under the card grinding appearance, the glass micropipette tip to be ground out required angle.
9. the preparation method of glass micropipette thermocouple according to claim 1 is characterized in that, described metallic film is a biocompatibility metal, and thickness is that micron is to nanoscale.
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| CN201110372044.3A CN102522490B (en) | 2011-11-21 | 2011-11-21 | Preparation method for glass micro-needle thermocouple |
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| CN201110372044.3A CN102522490B (en) | 2011-11-21 | 2011-11-21 | Preparation method for glass micro-needle thermocouple |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106768445A (en) * | 2016-12-29 | 2017-05-31 | 北京航空航天大学 | A kind of quick response temperature thermocouple |
| CN108387320A (en) * | 2018-02-08 | 2018-08-10 | 北京航空航天大学 | A kind of permanent mold casting quick response temperature thermocouple |
| CN108414106A (en) * | 2018-02-08 | 2018-08-17 | 北京航空航天大学 | A kind of casting mould quick response temperature thermocouple |
| CN111076836A (en) * | 2019-12-12 | 2020-04-28 | 西安交通大学 | Metal-oxide type thin film thermocouple and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5411600A (en) * | 1992-06-03 | 1995-05-02 | Eastman Kodak Company | Ultrathin film thermocouples and method of manufacture |
| CN1357930A (en) * | 2000-12-08 | 2002-07-10 | 中国科学院长春光学精密机械与物理研究所 | New-type thermocouple produced by means of photoetching techn and gas-phase deposition techn |
| CN101493360A (en) * | 2009-01-05 | 2009-07-29 | 东南大学 | Thermocouple with micron or nanometer grade tip curvature radius and method for producing the same |
-
2011
- 2011-11-21 CN CN201110372044.3A patent/CN102522490B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5411600A (en) * | 1992-06-03 | 1995-05-02 | Eastman Kodak Company | Ultrathin film thermocouples and method of manufacture |
| CN1357930A (en) * | 2000-12-08 | 2002-07-10 | 中国科学院长春光学精密机械与物理研究所 | New-type thermocouple produced by means of photoetching techn and gas-phase deposition techn |
| CN101493360A (en) * | 2009-01-05 | 2009-07-29 | 东南大学 | Thermocouple with micron or nanometer grade tip curvature radius and method for producing the same |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106768445A (en) * | 2016-12-29 | 2017-05-31 | 北京航空航天大学 | A kind of quick response temperature thermocouple |
| CN106768445B (en) * | 2016-12-29 | 2018-10-30 | 北京航空航天大学 | A kind of quick response temperature thermocouple |
| CN108387320A (en) * | 2018-02-08 | 2018-08-10 | 北京航空航天大学 | A kind of permanent mold casting quick response temperature thermocouple |
| CN108414106A (en) * | 2018-02-08 | 2018-08-17 | 北京航空航天大学 | A kind of casting mould quick response temperature thermocouple |
| CN108414106B (en) * | 2018-02-08 | 2019-07-12 | 北京航空航天大学 | A kind of casting mould quick response temperature thermocouple |
| CN111076836A (en) * | 2019-12-12 | 2020-04-28 | 西安交通大学 | Metal-oxide type thin film thermocouple and preparation method thereof |
| CN111076836B (en) * | 2019-12-12 | 2020-10-27 | 西安交通大学 | Metal-oxide type thin film thermocouple and preparation method thereof |
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| CN102522490B (en) | 2014-02-26 |
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