CN203525984U - Spin coater with pre-annealing function - Google Patents
Spin coater with pre-annealing function Download PDFInfo
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- CN203525984U CN203525984U CN201320623449.4U CN201320623449U CN203525984U CN 203525984 U CN203525984 U CN 203525984U CN 201320623449 U CN201320623449 U CN 201320623449U CN 203525984 U CN203525984 U CN 203525984U
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- glue
- water
- annealing
- spin coater
- evenning machine
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Abstract
The patent discloses a spin coater with a pre-annealing function. The spin coater comprises four parts including a glue injecting device, a heating device, a heat radiating device and a spin coater body, wherein the glue injecting device simplifies a manual glue dropping process into a control process of simple switching action of a normally-closed-type water valve, thus improving the glue dropping efficiency, and preventing problems possibly brought about by experience-based glue dropping; the heating device is used for heating samples and realizing the function of low-temperature pre-annealing of films; the heat radiating device is used for reducing the temperature of an inner container of the spin coater, accelerating the exchange of heat and gases inside and outside the heating device, and discharging organic substances escaping after heating; the spin coater body is used for realizing the glue spinning operation in the preparing of films. The device provided by the utility model can simplify the experiment flow for preparing films by glue dissolving, glue dropping by a gel method, glue spinning and low-temperature pre-annealing into the experiment flow for preparing films by repeated glue dropping, glue spinning and concentrated high-temperature thermal treatment by a rapid annealing furnace after low-temperature pre-annealing, and can shorten the film preparing time, and improve the film preparation efficiency greatly.
Description
Technical field
This patent relates to a kind of sol evenning machine, particularly a kind of sol evenning machine with preannealing function.
Background technology
The advantages [document one sees reference] such as sol-gel process is a kind of important thin-film material preparation means, possesses synthesis temperature low, and doping is convenient, and experiment condition is controlled flexibly, with low cost.This method generally need to be used sol evenning machine (for precursor solution is spun to substrate slice) and quick anneal oven (for the heat treatment of print), need to manually drip the experimentations [document two sees reference] such as glue, whirl coating, Low Temperature Thermal annealing, high-temperature thermal annealing.In its tradition application, this method exists the following improvements for the treatment of.
First needing improved is a manual glue spin coating operating process.In each heat treated Cheng Qian, need to use glue head dropper to draw colloidal sol and ooze a little to substrate slice, use sol evenning machine to complete whirl coating and film.The process of repeatedly draw colloidal sol, dripping glue seems simply, and actual needs expends part-time, and has certain empirical.Especially for needs, use sol-gel process to prepare in batches sample strip, the film of required growth relate to thickness thicker, need to carry out hundreds of time and even thousands of times drip glue, spin coating operation time, may there is certain problem.Such as each position of dripping glue needs naked eyes judgement; Dripping glue amount can not guarantee at every turn all accurately consistent; Manual operation expends man-hour etc. for a long time.
On the other hand, in thermal anneal process process, need to improve.Sol-gal process need to carry out thermal anneal process to the film after every layer of whirl coating, to realize the successively growth of material, finally reaches required film thickness.The shortcoming of this process is, when in solvent, the solubility of slaine is lower, the thickness that makes every layer film is less, often needs just can prepare the rete of desired thickness through glue-whirl coating-Low Temperature Thermal annealing-high-temperature thermal annealing cycle of dripping many times.For example, when using sol-gel process to prepare manganese cobalt-nickel oxide film, need to prepare film guarantee its lower square resistance and infrared Absorption that 6-10 μ m is thick, to utilize its sensitive characteristic to realize infra-red heat, survey.And during actual fabrication, because the concentration of the acetate solution of manganese, cobalt, nickel is lower, each whirl coating can only obtain the film that about 22nm is thick, with the film thickness gauge of 8 μ m, need to repeat just can make for approximately 360 times [document three, four sees reference].If each masking cycle cost 15 minutes, completing film making needs 90 hours, i.e. on more than ten working days, efficiency is comparatively low.If can carry out the processing of low temperature preannealing after each films the cycle, after can repeated multiple timesly filming, concentrate annealing, so can greatly shorten the masking time.
This patent, by the simple switch action control of closed type water valve, is realized the process of automatic glue-dropping, whirl coating; Utilize contact switch to control the power of infrared lamp, realize the preannealing process of film sample; Adopting heat abstractor is the cooling of sol evenning machine inner bag, and promotes the exchange heat that heater is inside and outside, realizes thermal balance.This patent has overcome and has manually drawn colloidal sol-drip the empirical problem that glue operation may bring, and greatly shortens the masking time, has improved masking efficiency.
The list of references more than relating to is as follows:
1.Hou,Y.,et?al.,Characterization?of?Mn(1.56)Co(0.96)Ni(0.48)O(4)films?for?infrared?detection.Applied?Physics?Letters,2008.92(20).
2. Hou Yun, Huang Zhiming etc., the preparation method of manganese-cobalt-nickel thin film heat-sensitive material. patent of invention, 2007.
3. Ge Yu builds, chemical deposition low-temperature epitaxy manganese-cobalt-nickel thin film crystallinity and infrared spectroscopic ellipsometry research. infrared and millimeter wave journal, 2008.27:p.413.
4. Ge Yu builds, the preparation characterization of manganese cobalt-nickel oxide film and device research. thesis for the doctorate, 2008.
Summary of the invention
This patent provides a kind of film of can repeatedly filming-dry, and has the sol evenning machine of preannealing function, has overcome and has manually dripped the empirical of glue operation, has solved the inefficient problem of sol-gel process masking.
A kind of concrete structure of the sol evenning machine with preannealing function as shown in Figure 1, comprises glue filling device, heater, heat abstractor and sol evenning machine four parts.
Described glue filling device comprises take lower member: glass dropper 3, normally closed type water valve 5, Y-type three way type 6, precise manual lifting platform and precise manual two-dimension translational platform 7, liquid storage bottle 8 and the counterweight 9 of two ZQW one-way water stop valves 4,12 that model is 3WY-35-012,60ml medical grade rubber piston plastic injector 11, the medical frosted matter of 60ml glass syringe 10,15ml.
Described heater is mainly by forming with lower member: the infrared lamp 14 of power 275W; Model is the contact switch 15 of KW12-3Z-18; Model is Panasonic's relay 16 of JQ1-DC12V-F; 10k Ω current-limiting resistance 17; Two joint 6V battery 18 and 220V alternating voltages 22.
Described heat abstractor is mainly by forming with lower member: the heat dissipation copper pipe 13 of diameter 8mm, be of a size of 154 (L) * 118 (W) * 30 (H) mm
3water of radiation row 19(comprise aluminum heat radiation row and 12V DC fan), water storage case 20 and QD type single-plase submerged pump 21.
Described sol evenning machine 1 adopts Beijing Xin Youyan company KW-4A type sol evenning machine that produce, that suction nozzle 2 is housed.
Described sol evenning machine 1 is for stationary substrate sheet spin coating colloidal sol; Sol evenning machine 1 left side is glue filling device, piston plastic injector 11 and frosted matter glass syringe 10 are used for respectively drawing and depositing colloidal sol, Y-type three way type 6 connects the first one-way water stop valve 4, normally closed type water valve 5, liquid storage bottle 8, frosted matter glass syringe 10, piston plastic injector 11 and the second one-way water stop valve 12, utilizes two one-way water stop valves to control liquid flow direction; Dropper 3 is fixed on two-dimension translational platform, utilizes lifting platform and two-dimension translational platform 7 to control the orientation of glue dropping hole; On the push rod of frosted matter glass syringe 10, add the counterweight 9 of approrpiate wts, rely on the gravity of counterweight 9 that push rod is pressed down, thereby colloidal sol is dropwise expressed on substrate slice from dropper; Utilize emulsion tube to connect Y-type three way type 6 and first one-way water stop valve 4 two parts, and at centre design normally closed type water valve 5, the glue process of dripping of the on off state capable of controlling dropping pipe by manual adjustments normally closed type water valve 5;
Sol evenning machine 1 top is heater, with 220V alternating current 22, provide voltage for 275W infrared lamp 14, by contact switch 15, relay 16 and current-limiting resistance 17, control the actual power of infrared lamps, and then the Pre-annealing Temperature of Quality control, realize the preannealing function of film; Infrared lamp 22 near time, contact switch 15 closures, current-limiting resistance 17 is by short circuit, it is maximum that infrared lamp 22 power reach, substrate surface temperature can reach 230-250 ℃, the organic substance in institute's coated film will all be overflowed or burnout in tens of seconds; Infrared lamp 22 away from time, contact switch 15 disconnects, current-limiting resistance 17 accesses, infrared lamp 22 power reductions are dimmed, can be coated with membrane operations;
Glue filling device right side is heat abstractor, and water storage case 20 is for storing heat radiation water, and immersible pump 21 circulates water in copper pipe; Cooling water is lowered the temperature for sol evenning machine inner bag by the flow through heat dissipation copper pipe 13 that is surrounded on inner bag of immersible pump 21, through water of radiation row 19, the heat of inner bag is scattered, thereby water is lowered the temperature, and promote heat and the gas exchange that heater is inside and outside, discharge the organic substance of overflowing after heating.
This patent has the following advantages: drip glue, whirl coating and the low temperature heat treatment of sol-gel process are combined, adopt and repeatedly repeat with quick anneal oven, to concentrate the mode of high-temperature heat treatment to prepare film after glue-whirl coating-low temperature preannealing; Use glue head dropper is drawn to the manual processes of colloidal sol, a glue, be reduced to the process of the simple switch action control of closed type water valve, improved a glue efficiency, avoid the problem that glue action may bring of dripping of empirical; The film preparation flow process of having simplified sol-gel process, has improved masking efficiency greatly.
Accompanying drawing explanation
The side view of the sol evenning machine that Fig. 1 this patent relates to, in figure: 1, sol evenning machine 2, suction nozzle 3, dropper 4, the first one-way water stop valve 5, normally closed type water valve 6, Y-type three way type, 7, lifting platform and two-dimension translational platform 8, liquid storage bottle 9, counterweight 10, frosted matter glass syringe 11, piston plastic injector 12, the second one-way water stop valve 13, heat dissipation copper pipe 14, infrared lamp 15, contact switch 16, relay 17, current-limiting resistance 18, battery 19, water of radiation row 20, water storage case 21, immersible pump 22, AC power.
The specific embodiment
Examples of implementation
1. prepare precursor solution.To target components, be Mn
1.56co
0.96ni
0.48o
4mn oxide, take respectively four water acetic acid manganese 91.76g, Cobalt diacetate tetrahydrate 57.39g, four water acetic acid nickel 28.66g, add the ratio of 400ml acetic acid, 100ml water that powder is dissolved according to every 100g acetate, pour in the solution splendid attire ware of negative pressure leaching machine, selecting aperture is the filter membrane of 0.45 μ m, carry out negative pressure leaching, the contamination precipitation in filtering solution, obtains Mn
1.56co
0.96ni
0.48o
4precursor solution, and it is standby to pack solution into liquid storage bottle.
2. prepare manganese cobalt nickel oxygen film.Adopt this sol evenning machine device at aluminium oxide (Al
2o
3) prepare Mn on substrate
1.56co
0.96ni
0.48o
4film, after each spin coating, utilizes its self-heating apparatus to carry out heating, drying (drying 1min at～250 ℃) to film, uses quick anneal oven (RTP-500) instead at 750 ℃ of annealing 2min after repeating to drip glue, spin coating 6 times.Repeat above-mentioned steps 9 times, make the film that thickness is about 1.0 μ m.
3, annealing.Use Muffle furnace at 750 ℃ of annealing 3h the film preparing, gained manganese cobalt nickel oxygen film morphology, crystallinity and thermo-sensitive property and the sol-gel process preparation-obtained film of successively annealing is substantially suitable, and its room temperature (300K) temperature-coefficient of electrical resistance reaches α=-3.5%/K.
Claims (1)
1. a sol evenning machine with preannealing function, comprises glue filling device, heater, and heat abstractor and sol evenning machine four parts, is characterized in that:
Described sol evenning machine (1) is for stationary substrate sheet spin coating colloidal sol; Sol evenning machine (1) left side is glue filling device, piston plastic injector (11) and frosted matter glass syringe (10) are used for respectively drawing and depositing colloidal sol, Y-type three way type (6) connects the first one-way water stop valve (4), normally closed type water valve (5), liquid storage bottle (8), frosted matter glass syringe (10), piston plastic injector (11) and the second one-way water stop valve (12), utilize two one-way water stop valves (4,12) to control liquid flow direction; Dropper (3) is fixed on two-dimension translational platform, utilizes lifting platform and two-dimension translational platform (7) to control the orientation of glue dropping hole; On the push rod of frosted matter glass syringe (10), add the counterweight (9) of approrpiate wts, rely on the gravity of counterweight (9) that push rod is pressed down, thereby colloidal sol is dropwise expressed on substrate slice from dropper; Utilize emulsion tube to connect Y-type three way type (6) and the first one-way water stop valve (4) two parts, and at centre design normally closed type water valve (5), a glue process of the on off state capable of controlling dropping pipe by manual adjustments normally closed type water valve (5);
Sol evenning machine (1) top is heater, with 220V alternating current (22), for 275W infrared lamp (14), provide voltage, by contact switch (15), relay (16) and current-limiting resistance (17), control the actual power of infrared lamp, and then the Pre-annealing Temperature of Quality control, realize the preannealing function of film; When infrared lamp (22) is close, contact switch (15) closure, current-limiting resistance (17) is by short circuit, and it is maximum that infrared lamp (22) power reaches, substrate surface temperature can reach 230-250 ℃, and the organic substance in institute's coated film will all be overflowed or burnout in tens of seconds; Infrared lamp (22) away from time, contact switch (15) disconnects, current-limiting resistance (17) access, infrared lamp (22) power reduction is dimmed, can be coated with membrane operations;
Glue filling device right side is heat abstractor, and water storage case (20) is for storing heat radiation water, and immersible pump (21) circulates water in copper pipe; Cooling water is the cooling of sol evenning machine inner bag by immersible pump (21) heat dissipation copper pipe (13) that is surrounded on inner bag of flowing through, through water of radiation row (19), the heat of inner bag is scattered, thereby water is lowered the temperature, and promote heat and the gas exchange that heater is inside and outside, discharge the organic substance of overflowing after heating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320623449.4U CN203525984U (en) | 2013-10-10 | 2013-10-10 | Spin coater with pre-annealing function |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320623449.4U CN203525984U (en) | 2013-10-10 | 2013-10-10 | Spin coater with pre-annealing function |
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| CN203525984U true CN203525984U (en) | 2014-04-09 |
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| CN201320623449.4U Withdrawn - After Issue CN203525984U (en) | 2013-10-10 | 2013-10-10 | Spin coater with pre-annealing function |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103495529A (en) * | 2013-10-10 | 2014-01-08 | 中国科学院上海技术物理研究所 | Glue mixing machine with pre-annealing function |
-
2013
- 2013-10-10 CN CN201320623449.4U patent/CN203525984U/en not_active Withdrawn - After Issue
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103495529A (en) * | 2013-10-10 | 2014-01-08 | 中国科学院上海技术物理研究所 | Glue mixing machine with pre-annealing function |
| CN103495529B (en) * | 2013-10-10 | 2016-01-13 | 中国科学院上海技术物理研究所 | A kind of sol evenning machine with preannealing function |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20140409 Effective date of abandoning: 20160113 |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20140409 Effective date of abandoning: 20160113 |
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| C25 | Abandonment of patent right or utility model to avoid double patenting |