CN108558430A - A kind of manufacture craft of Low emissivity aerogel film - Google Patents
A kind of manufacture craft of Low emissivity aerogel film Download PDFInfo
- Publication number
- CN108558430A CN108558430A CN201810542417.9A CN201810542417A CN108558430A CN 108558430 A CN108558430 A CN 108558430A CN 201810542417 A CN201810542417 A CN 201810542417A CN 108558430 A CN108558430 A CN 108558430A
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- Prior art keywords
- film
- aerogel
- water
- colloidal sol
- gel
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
Abstract
The invention discloses a kind of manufacture crafts of Low emissivity aerogel film, include the following steps：Colloidal sol preparation, film preparation, heat treatment, performance test, is packaged encapsulation at colloidal sol processing, and by the Low emissivity aerogel film of this technique productions, first, being formd using acid/base two-step catalysis process, structure is more loose while gel network but also with some strength；Second is that using the solvent of low surface tension as final solvent so that the structure both shrinks degree caused by the capillary tension that gel mould is generated by solvent volatilization in the drying process reduces, and then maintains higher hole ratio；Third, having carried out silanization process to micelle surface, pass through Si (CH3)3Group is instead of the H in micelle surface OH groups, realize that film structure after dry shrink rebounds again, the original porous structure of gel is utmostly maintained, while aeroge is modified by heat treatment, the radiation resistance through the 300 DEG C and 600 DEG C modified aeroges of heat treatment is preferable.
Description
Technical field
The present invention relates to aerogel film technical field, specially a kind of manufacture craft of Low emissivity aerogel film.
Background technology
Aeroge is a kind of novel nano-porous materials, is that a kind of lightweight nanometer that solar heat protection heat-proof quality is very outstanding is more
Hole amorphous solid material, porosity are up to 80-99.8%, and the typical sizes of hole are 1-100nm, specific surface area 200-
1000m2/g, and density can be down to 3kg/m3, room temperature thermal coefficient can be down to 0.012W/ (mk), just because of these features
Aerogel material is set to have very wide application potential, aerogel in terms of calorifics, acoustics, optics, microelectronics, particle detection
Technology is further to expand the application of aeroge, aerogel have the application of bulk silicon dioxide aeroge as much it
Outside, also its unique performance；With structure-controllable, refractive index is adjustable, and dielectric constant is small, and stability is good, has had with silicon viscous
The clearance filling capability that attached property is become reconciled, that there are porositys is low for the manufacture craft of existing aerogel film, while aerogel is anti-
Radianting capacity is weaker, is unfavorable for using.
Invention content
The present invention provides a kind of manufacture craft of Low emissivity aerogel film, can effectively solve asking in above-mentioned background technology
Topic.
To achieve the above object, the present invention provides the following technical solutions：A kind of manufacture craft of Low emissivity aerogel film, packet
Include following steps：
1. a kind of manufacture craft of Low emissivity aerogel film, includes the following steps：
One, colloidal sol is prepared
Colloidal sol is prepared using colloidal sol-gel process of acid/base two-step catalysis；
Ethyl orthosilicate TEOS, deionized water H2O, absolute ethyl alcohol Eth and hydrochloric acid HCl are pressed 1:1.5:25:0.0007
Molar ratio mixes, and in 60 DEG C of hydrolysis/condensation reaction 90min and is stirred continuously using heating water bath, obtained solution is known as mother
Liquid；
2) mixed liquor of 18mL ethyl alcohol and 1mL0.05M ammonium hydroxide NH4OH is slowly added into 36mL mother liquors, and in room temperature
Under be stirred continuously 30min. and obtain mixed solution, operated to following steps：
Two, colloidal sol is handled
Colloidal sol obtained above is placed in 50 DEG C of air aging and gelation, after 4 days, colloidal sol is transformed into gel, connects
It and carries out cleaning and silanization, after the completion of cleaning and silanization, add suitable normal heptane weighing apparatus and release gel and sonic oscillation, when
Gel shake again broken colloidal sol for mobility when, you can be used for the preparation of aerogel；
Three, film preparation
Using single crystalline Si piece as substrate, film is prepared using spin-coating method, speed of rotation 2000rpm, time 20s are thin
For film through 450 DEG C of annealing 60min, heating and rate of temperature fall are 8 DEG C/min, repeat the above process the gas that can be obtained required thickness
Gel film；
Four, it is heat-treated
The aerogel that step 3 obtains is heat-treated in atmosphere, heat treatment temperature is 100~400 DEG C, is risen
Warm rate is 2,5~10 DEG C/min, and soaking time is 1~10h, and last natural cooling obtains modified aerogels film；
Five, performance test
The infrared characteristic that modified aerogels film is analyzed with FTIR observes film using bare silicon wafer as piece is accompanied using SEM
The optical constant in surface topography and section, film is then measured by elliptical polarization spectroscopy；
Six, it is packaged encapsulation
The qualified aerogel film that step 5 obtains is subjected to secondary detection, the aerogel film after detection is qualified is packaged
Encapsulation is put in storage after the completion of encapsulation.
According to above-mentioned technical proposal：The cleaning method of the step 2 colloidal sol processing is, first by soak to sewage second
It is cleaned in alcohol, removes acidand basecatalysts undesired impurities.
According to above-mentioned technical proposal：The Silicane Method of the step 2 colloidal sol processing is, by the gel after cleaning with just
Heptane replaces the alcohol solvent in gel network structure, and gel is then dipped in the normal heptane of 5% volume containing trim,ethylchlorosilane
The silanization on micelle surface is carried out in solution.
According to above-mentioned technical proposal：The operating procedure of colloidal sol preparation immersion method is in the step 1:
1) inlet valve to be opened, water is made to enter cylinder, when arriving certain liquid level, overflow pipe water outlet determines that water has been filled it up in cylinder,
It is then shut off inlet valve；
2) it is first turned on power switch, starts water pump, " automatic/hand " switching switch is then allocated to " automatic " at this time
" heating operation " indicator light is bright, and electrothermal tube is begun to warm up, when water temperature reaches setting ceiling temperature in cylinder, " heating operation " instruction
Lamp extinguishes, and " heating stops " indicator light is bright, and electrothermal tube does not heat, and at this moment, can heat cryogenic natural gas；
3) intake valve and air outlet valve are slowly opened successively, close by-passing valve；
4) when heater works, SEA LEVEL VARIATION is often observed, water level will be replenished in time when being less than lower limit；
5) when stopping using water-bath type heater, by-passing valve is slowly opened, closes intake valve, air outlet valve；
6) cut off the water pump, close the power switch of water-bath type heater, open cylinder and put clear valve, put the water in clear cylinder.
According to above-mentioned technical proposal：After if the heating water bath is used for a long time, the automatic heating line failure of electric control gear, no
It can work normally, " automatic/hand " can be switched switch at this time be allocated to " manual ", then operate manual open and close button, this work
Under state, digital display meter display barrel body temperature, it is necessary to temperature in manual operation application cylinder, the general upper limit not across 70 DEG C, under
Limit is not less than 30 DEG C, while must repair automatic heating line as early as possible.
According to above-mentioned technical proposal：Spin-coating method is in the step 3 film preparation：A, equably by the coagulant liquid of atomization
It is sprayed on substrate, then driving substrate rotates the coagulant liquid formation film layer so that on substrate, stops after coagulant liquid distribution is stablized
The only rotation of substrate；B, injecting glue is carried out at the heart in the substrate, then drive substrate rotate coagulant liquid to center injecting glue it is uniformly distributed after
It stops rotating.
According to above-mentioned technical proposal：The step a and step b be carry out successively, reversed order carry out, or alternately repeatedly into
Row.
Compared with prior art, beneficial effects of the present invention：By the Low emissivity aerogel film of this technique productions, first, adopting
Form that structure is more loose while gel network but also with some strength with acid/base two-step catalysis process；Second is that using
The solvent of low surface tension is as final solvent so that the capillary tension that gel mould is generated by solvent volatilization in the drying process
Caused structure both shrinks degree reduces, and then maintains higher hole ratio；Third, having carried out silanization mistake to micelle surface
Journey passes through Si (CH3)3Group realizes that film structure after dry shrink rebounds again instead of the H in micelle surface OH groups,
The original porous structure of gel is utmostly maintained, while aeroge is modified by heat treatment, through 300 DEG C and 600
The radiation resistance of DEG C modified aeroge of heat treatment is preferable.
Description of the drawings
Attached drawing is used to provide further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.
In the accompanying drawings：
Fig. 1 is the flow diagram of the present invention.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment：As shown in Figure 1, the present invention provides a kind of manufacture craft of Low emissivity aerogel film, include the following steps：
A kind of manufacture craft of Low emissivity aerogel film, includes the following steps：
One, colloidal sol is prepared
Colloidal sol is prepared using colloidal sol-gel process of acid/base two-step catalysis；
Ethyl orthosilicate TEOS, deionized water H2O, absolute ethyl alcohol Eth and hydrochloric acid HCl are pressed 1:1.5:25:0.0007
Molar ratio mixes, and in 60 DEG C of hydrolysis/condensation reaction 90min and is stirred continuously using heating water bath, obtained solution is known as mother
Liquid；
2) mixed liquor of 18mL ethyl alcohol and 1mL0.05M ammonium hydroxide NH4OH is slowly added into 36mL mother liquors, and in room temperature
Under be stirred continuously 30min. and obtain mixed solution, operated to following steps：
Two, colloidal sol is handled
Colloidal sol obtained above is placed in 50 DEG C of air aging and gelation, after 4 days, colloidal sol is transformed into gel, connects
It and carries out cleaning and silanization, after the completion of cleaning and silanization, add suitable normal heptane weighing apparatus and release gel and sonic oscillation, when
Gel shake again broken colloidal sol for mobility when, you can be used for the preparation of aerogel；
Three, film preparation
Using single crystalline Si piece as substrate, film is prepared using spin-coating method, speed of rotation 2000rpm, time 20s are thin
For film through 450 DEG C of annealing 60min, heating and rate of temperature fall are 8 DEG C/min, repeat the above process the gas that can be obtained required thickness
Gel film；
Four, it is heat-treated
The aerogel that step 3 obtains is heat-treated in atmosphere, heat treatment temperature is 100~400 DEG C, is risen
Warm rate is 2.5~10 DEG C/min, and soaking time is 1~10h, and last natural cooling obtains modified aerogels film；
The infrared characteristic that modified aerogels film is analyzed with FTIR observes film using bare silicon wafer as piece is accompanied using SEM
The optical constant in surface topography and section, film is then measured by elliptical polarization spectroscopy；
Six, it is packaged encapsulation
The qualified aerogel film that step 5 obtains is subjected to secondary detection, the aerogel film after detection is qualified is packaged
Encapsulation is put in storage after the completion of encapsulation.
According to above-mentioned technical proposal：The cleaning method of the step 2 colloidal sol processing is, first by soak to sewage second
It is cleaned in alcohol, removes acidand basecatalysts undesired impurities.
According to above-mentioned technical proposal：The Silicane Method of step 2 colloidal sol processing is, by the gel normal heptane after cleaning
The alcohol solvent in gel network structure is replaced, gel is then dipped in the n-heptane solution of 5% volume containing trim,ethylchlorosilane
The middle silanization for carrying out micelle surface.
According to above-mentioned technical proposal：The operating procedure of colloidal sol preparation immersion method is in step 1:
1) inlet valve to be opened, water is made to enter cylinder, when arriving certain liquid level, overflow pipe water outlet determines that water has been filled it up in cylinder,
It is then shut off inlet valve；
2) it is first turned on power switch, starts water pump, " automatic/hand " switching switch is then allocated to " automatic " at this time
" heating operation " indicator light is bright, and electrothermal tube is begun to warm up, when water temperature reaches setting ceiling temperature in cylinder, " heating operation " instruction
Lamp extinguishes, and " heating stops " indicator light is bright, and electrothermal tube does not heat, and at this moment, can heat cryogenic natural gas；
3) intake valve and air outlet valve are slowly opened successively, close by-passing valve；
4) when heater works, SEA LEVEL VARIATION is often observed, water level will be replenished in time when being less than lower limit；
5) when stopping using water-bath type heater, by-passing valve is slowly opened, closes intake valve, air outlet valve；
6) cut off the water pump, close the power switch of water-bath type heater, open cylinder and put clear valve, put the water in clear cylinder.
According to above-mentioned technical proposal：After if heating water bath is used for a long time, the automatic heating line failure of electric control gear, Bu Nengzheng
" automatic/hand " can be switched switch at this time and be allocated to " manual ", then operate manual open and close button, this working condition by often work
Under, digital display meter display barrel body temperature, it is necessary to which temperature in manual operation application cylinder, the general upper limit is not across 70 DEG C, and lower limit is not
Less than 30 DEG C, while automatic heating line must be repaired as early as possible.
According to above-mentioned technical proposal：Spin-coating method is in step 3 film preparation：A, the coagulant liquid of atomization is equably sprayed
On substrate, then driving substrate rotates the coagulant liquid formation film layer so that on substrate, stops base after coagulant liquid distribution is stablized
The rotation of piece；B, injecting glue is carried out at the heart in the substrate, then drive substrate rotate coagulant liquid to center injecting glue it is uniformly distributed after stop
Rotation.
According to above-mentioned technical proposal：Step a and step b is to carry out successively, and reversed order carries out, or is alternately repeatedly carried out.
Based on above-mentioned, it is an advantage of the current invention that by the Low emissivity aerogel film of this technique productions, when using acid/
Alkali two-step catalysis process forms that structure is more loose while gel network but also with some strength；Second is that using low surface
The solvent of tension is as final solvent so that gel mould is in the drying process caused by the capillary tension that solvent volatilization generates
Structure both shrinks degree reduce, and then maintain higher hole ratio；Third, having carried out silanization process to micelle surface, pass through
Si(CH3)3Group realizes that film structure after dry shrink rebounds again, maximum journey instead of the H in micelle surface OH groups
Degree maintains the original porous structure of gel, while being modified to aeroge by heat treatment, at 300 DEG C and 600 DEG C heat
The radiation resistance for managing modified aeroge is preferable.
Finally it should be noted that：The foregoing is merely the preferred embodiments of the present invention, are not intended to restrict the invention, to the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, for those skilled in the art, still can be with
Technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.It is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in the guarantor of the present invention
Within the scope of shield.
Claims (7)
1. a kind of manufacture craft of Low emissivity aerogel film, it is characterised in that：Include the following steps：
One, colloidal sol is prepared：
1) ethyl orthosilicate, deionized water, absolute ethyl alcohol and hydrochloric acid are pressed 1:1.5:25:0.0007 molar ratio mixing, uses
Heating water bath reacts 90min at 60 DEG C and is stirred continuously, and obtained solution is known as mother liquor；
2) mixed liquor of 18mL ethyl alcohol and 1mL0.05M ammonium hydroxide is added in 36mL mother liquors, and 30min is stirred at room temperature, obtained
To mixed solution, as colloidal sol；
Two, colloidal sol is handled
Colloidal sol obtained above is placed in 50 DEG C of air aging and gelation, after 4 days, colloidal sol is transformed into gel, then into
Row cleaning and silanization add suitable normal heptane weighing apparatus and release gel and sonic oscillation, work as gel after the completion of cleaning and silanization
Again shake broken colloidal sol for mobility when, you can be used for the preparation of aerogel；
Three, film preparation
Using single crystalline Si piece as substrate, film, speed of rotation 2000rpm, time 20s, film warp are prepared using spin-coating method
450 DEG C of annealing 60min, heating and rate of temperature fall are 8 DEG C/min, repeat the above process the aeroge that can be obtained required thickness
Film；
Four, it is heat-treated
The aerogel that step 3 obtains is heat-treated, heat treatment temperature is 100~400 DEG C, heating rate 2,5~
10 DEG C/min, soaking time is 1~10h, and last natural cooling obtains modified aerogels film；
Five, performance test
The infrared characteristic that modified aerogels film is analyzed with FTIR observes the surface of film using SEM using bare silicon wafer as piece is accompanied
The optical constant in pattern and section, film is then measured by elliptical polarization spectroscopy；
Six, it is packaged encapsulation
The qualified aerogel film that step 5 obtains is subjected to secondary detection, the aerogel film after detection is qualified carries out packing envelope
Dress is put in storage after the completion of encapsulation.
2. a kind of manufacture craft of Low emissivity aerogel film according to claim 1, it is characterised in that：The step 2 is molten
The cleaning method of glue processing is that will first be cleaned in soak to sewage ethyl alcohol, removes acidand basecatalysts undesired impurities.
3. a kind of manufacture craft of Low emissivity aerogel film according to claim 1, it is characterised in that：The step 2 is molten
The Silicane Method of glue processing is the normal heptane of the gel after cleaning to be replaced the alcohol solvent in gel network structure, then
Gel is dipped in the silanization that micelle surface is carried out in the n-heptane solution of 5% volume containing trim,ethylchlorosilane.
4. a kind of manufacture craft of Low emissivity aerogel film according to claim 1, it is characterised in that：In the step 1
Colloidal sol prepare immersion method operating procedure be
1) inlet valve is opened, water is made to enter cylinder, when arriving certain liquid level, overflow pipe water outlet determines that water has been filled it up in cylinder, then
Close inlet valve；
2) it is first turned on power switch, starts water pump, " automatic/hand " switching switch is then allocated to " automatic " " heating at this time
Operation " indicator light is bright, and electrothermal tube is begun to warm up, and when water temperature reaches setting ceiling temperature in cylinder, " heating operation " indicator light is put out
It goes out, " heating stops " indicator light is bright, and electrothermal tube does not heat, and at this moment, can heat cryogenic natural gas；
3) intake valve and air outlet valve are slowly opened successively, close by-passing valve；
4) when heater works, SEA LEVEL VARIATION is often observed, water level will be replenished in time when being less than lower limit；
5) when stopping using water-bath type heater, by-passing valve is slowly opened, closes intake valve, air outlet valve；
6) cut off the water pump, close the power switch of water-bath type heater, open cylinder and put clear valve, put the water in clear cylinder.
5. a kind of manufacture craft of Low emissivity aerogel film according to claim 4, it is characterised in that：The heating water bath
If after being used for a long time, the automatic heating line failure of electric control gear, cisco unity malfunction can switch " automatic/hand " open at this time
Pass is allocated to " manual ", then operates manual open and close button, under this working condition, digital display meter display barrel body temperature, it is necessary to people
Temperature in work operation and control cylinder, for the general upper limit not across 70 DEG C, lower limit is not less than 30 DEG C, while must repair automatic heating as early as possible
Circuit.
6. a kind of manufacture craft of Low emissivity aerogel film according to claim 1, it is characterised in that：The step 3 is thin
Spin-coating method is in film preparation：A, the coagulant liquid of atomization is equably sprayed on substrate, then drives substrate rotation so that substrate
On coagulant liquid formed film layer, after coagulant liquid distribution stablize after stop substrate rotation；B, injecting glue is carried out at the heart in the substrate, so
Afterwards driving substrate rotate the coagulant liquid to center injecting glue it is uniformly distributed after stop rotating.
7. a kind of manufacture craft of Low emissivity aerogel film according to claim 6, it is characterised in that：The step a and
Step b is to carry out successively, and reversed order carries out, or is alternately repeatedly carried out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810542417.9A CN108558430A (en) | 2018-05-30 | 2018-05-30 | A kind of manufacture craft of Low emissivity aerogel film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810542417.9A CN108558430A (en) | 2018-05-30 | 2018-05-30 | A kind of manufacture craft of Low emissivity aerogel film |
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| Publication Number | Publication Date |
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| CN108558430A true CN108558430A (en) | 2018-09-21 |
Family
ID=63540881
Family Applications (1)
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|---|---|---|---|
| CN201810542417.9A Pending CN108558430A (en) | 2018-05-30 | 2018-05-30 | A kind of manufacture craft of Low emissivity aerogel film |
Country Status (1)
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544324A (en) * | 2003-11-20 | 2004-11-10 | 中国科学院上海技术物理研究所 | Silica dioxide aerogel membrane material preparation method |
| CN101774592A (en) * | 2009-10-31 | 2010-07-14 | 华南理工大学 | High heat insulation transparent SiO2 aerogel film material and preparation method thereof |
| CN104646248A (en) * | 2015-01-28 | 2015-05-27 | 天津森普捷科技有限公司 | Method and device for preparing thin film materials by spin-coating method |
-
2018
- 2018-05-30 CN CN201810542417.9A patent/CN108558430A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544324A (en) * | 2003-11-20 | 2004-11-10 | 中国科学院上海技术物理研究所 | Silica dioxide aerogel membrane material preparation method |
| CN101774592A (en) * | 2009-10-31 | 2010-07-14 | 华南理工大学 | High heat insulation transparent SiO2 aerogel film material and preparation method thereof |
| CN104646248A (en) * | 2015-01-28 | 2015-05-27 | 天津森普捷科技有限公司 | Method and device for preparing thin film materials by spin-coating method |
Non-Patent Citations (1)
| Title |
|---|
| TFYWXB4: "《水浴式加热器操作规程》", 21 March 2015 * |
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Application publication date: 20180921 |