CN103796346A - High-temperature nano-electrothermal film of double-film structure and preparation method thereof - Google Patents
High-temperature nano-electrothermal film of double-film structure and preparation method thereof Download PDFInfo
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Abstract
A high-temperature nano-electrothermal film of a double-film structure is composed of a quartz substrate, an alloy film electrode and a silicon carbide and molybdenum disilicide composite film layer. By means of a method of magnetron sputtering, first the alloy film electrode is arranged on the quartz substrate in a mask sputtering mode, then a silicon carbide film layer and a molybdenum disilicide film layer sequentially deposit; finally, high temperature annealing is conducted, and the surface of the molybdenum disilicide film layer is oxidized into a thin silicon dioxide protective layer. The alloy film electrode is a platinum alloy film electrode or a cobalt-base alloy film electrode. Two types of high temperature nanometer materials including silicon carbide and molybdenum disilicide with the purity of 99.950% are adopted in the electrothermal film, the surface of the film layer is oxidized to a silicon dioxide polycrystalline structure, oxygen is isolated, the service life of the electrothermal film is effectively prolonged, and the safety factor is effectively improved. The advantages of the two materials are utilized by the high-temperature nano-electrothermal film, work temperature is as high as 1000 DEG C, meanwhile heat efficiency is 98% or so, and the high-temperature nano-electrothermal film can be widely applied to the technical field of high temperature heating and the like.
Description
Technical field
The present invention relates to high-temperature nano Electric radiant Heating Film of a kind of double membrane structure and preparation method thereof, belong to semiconductor heating and Infrared Radiation Technology field.
Background technology
Along with the tellurian energy is day by day exhausted, energy-saving and emission-reduction more and more become the topic of social concerns, improve energy utilization rate particularly important.The mode of heating of common electric heater has the mode such as Resistant heating, electromagnetic radiation heating in the market.For Resistant heating, have the defects such as the heat efficiency is low, coefficient of safety is low, later maintenance cost is high, the life-span is short, and also there is harm and the cost high defect of electromagnetic radiation to human body in Electromagnetic Heating, has therefore occurred the heater element of many Electric radiant Heating Film types.It is a kind of typical planar heating element, has the advantages such as the heat efficiency is high, the flames of anger, homogeneous heating, corrosion-resistant, programming rate is fast, coefficient of safety is high, power attenuation amplitude can be ignored.Patent No. CN101668359A(title: a kind of Electric radiant Heating Film and manufacture method thereof, publication date: patent of invention 20100310) discloses a kind of composite metal electrothermal film heater element of single-layer membrane structure, this Electric radiant Heating Film composition and ratio (mass fraction) is: A: butter of tin, 5-10; B: titanium tetrachloride, 2-8; C: four nickel chlorides, 2-8; D: titanium trichloride, 2-8; E: ferric trichloride, 20-45; F: trichloride antimony, 0.5-0.8; G: U-Ramin MC, 0.5-0.8; H: potassium chloride, 1-4; I: caddy, 2-7; J: tin ash, 3-10; K: four tin oxide, 5-15; L: hydrofluoric acid, 3-8; M: boric acid, 0.2-1; N: ethanol, 5-15; O: isopropyl alcohol, 4-8; P: inorganic water, 20-45; This Electric radiant Heating Film complicated component, structure is single, and working temperature can only reach 500 ℃, and desired power is very high, and the heat efficiency is low in addition, and this has just limited the extensive use of electrothermal membrane heating element.
Summary of the invention
The present invention is directed to the problems referred to above and disclose high-temperature nano Electric radiant Heating Film of a kind of double membrane structure of good stability and preparation method thereof, maximum feature is the advantage that combines carborundum and molybdenum disilicide, has avoided their intrinsic defects simultaneously.By to the heating combination of basic material and the optimization of process conditions, can effectively overcome Electric radiant Heating Film prepared by prior art exists working temperature not high, and the power requiring is high, the defects such as the heat efficiency is low, Electric radiant Heating Film prepared by the present invention, can not only meet the condition of work of 1000 ℃, and can reach 98% the heat efficiency, the Electric radiant Heating Film function admirable of preparation.
Technical solution of the present invention is achieved in that
A high-temperature nano Electric radiant Heating Film for double membrane structure, is made up of quartz substrate, alloy firm electrode, carborundum and molybdenum disilicide composite film; Utilize the method for magnetron sputtering, mask sputter alloy firm electrode in quartz substrate, difference depositing silicon carbide rete and molybdenum disilicide rete in the substrate that is coated with alloy firm electrode; The oxidation of molybdenum disilicide film surface is formed to thin silicon dioxide layer of protection; Wherein said sputtering particle is nanoscale, and the thickness of described carborundum and molybdenum disilicide composite film is nanoscale.
Described alloy firm electrode is platinum alloy membrane electrode or cobalt-based alloy thin film electrode.
Carborundum purity in described silicon carbide film layer is 99.950%; In described molybdenum disilicide rete, molybdenum disilicide purity is 99.950%.
Described quartz substrate is resistant to elevated temperatures quartz plate or quartz ampoule, or is shaped as the high temperature resistant quartz substrate of curved surface.
A preparation method for the high-temperature nano Electric radiant Heating Film of double membrane structure, utilizes the method for magnetron sputtering, first mask sputter alloy firm electrode in quartz substrate, and then depositing silicon carbide rete, then deposit molybdenum disilicide rete, thus obtain double membrane structure; Concrete steps are as follows:
A) in the quartz substrate that is coated with alloy firm electrode by carborundum and molybdenum disilicide, adopt successively the mode plated film of rf magnetron sputtering; Described rf frequency is 13.56MHz; Sputtering chamber base vacuum degree is 2e-4Pa～5e-3Pa, and being at least 99.99% argon gas take purity is working gas, operating air pressure 1Pa, and flow 80sccm, target spacing is 80mm, sputtering power is 200W, 500 ℃ of quartz substrate temperature when sputter, negative substrate bias 20V;
B) under mixed atmosphere, adopt high annealing oxidation technology, by the oxidation of molybdenum disilicide film surface, form thin silicon dioxide layer of protection; Annealing temperature is 980 ℃, and annealing mixed atmosphere optimal proportion is argon gas, the nitrogen of volume fraction 15%-25% and the oxygen of volume fraction 10%-15% of volume fraction 60%-75%, annealing time 4h.
Advantage of the present invention and good effect are as follows:
1. planar heating can increase and the contact area of heated medium, obviously shortens heating time, and the heat efficiency, up to 98%, can improve effective utilization rate of energy simultaneously, is beneficial to sustainable development.
2. structure of the present invention provides two alloy firm electrodes, can serve as the electrothermal membrane heating element of 1000 ℃ of high temperature, can be applicable to high-temperature heat treatment field.
3. the combination of carborundum-molybdenum disilicide laminated film is conducive to bring into play the inherent characteristic of each comfortable high temperature heating, can avoid the at high temperature oxidizable and poor defect of molybdenum disilicide Toughness of carborundum simultaneously.
4. in anneal oxidation process, laminated film can form fine and close polycrystalline structure, and molybdenum disilicide surface is oxidized to silicon dioxide, has stopped that under top layer, molybdenum disilicide is further oxided.Superficial layer there will be free molybdenum element simultaneously, permeates each other in addition at carborundum-molybdenum disilicide contact-making surface, and this series of material structure characteristic all can effectively regulate the resistivity of this conductive composite film, is convenient to power control.
The advantages such as the present invention also has the flames of anger, homogeneous heating, corrosion-resistant, programming rate is fast, coefficient of safety is high, power attenuation amplitude can be ignored.
Accompanying drawing explanation
Fig. 1 is the Electric radiant Heating Film structural representation that the embodiment of the present invention 1 adopts platinum alloy membrane electrode to prepare;
Fig. 2 is the Electric radiant Heating Film structural representation that the embodiment of the present invention 2 adopts cobalt-based alloy thin film electrode to prepare;
Fig. 3 is the Electric radiant Heating Film work schematic diagram that adopts platinum alloy membrane electrode to prepare.
1, platinum alloy membrane electrode, 2, quartz substrate, 3, cobalt-based alloy thin film electrode, 4, silicon carbide film layer, 5, molybdenum disilicide rete, 6, silicon dioxide layer of protection.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.But the present embodiment can not be used for limiting the present invention, all employings similarity method of the present invention and similar variation thereof, all should list protection scope of the present invention in.
A high-temperature nano Electric radiant Heating Film for double membrane structure, as shown in Figure 1, by platinum alloy membrane electrode 1, quartz substrate 2, silicon carbide film layer 4, molybdenum disilicide rete 5 forms.Described quartz substrate is resistant to elevated temperatures quartz plate or quartz ampoule, or is shaped as the high temperature resistant quartz substrate of curved surface.
The preparation method of the high-temperature nano Electric radiant Heating Film of double membrane structure, its step is as follows:
Substrate is cleaned: quartz substrate utilizes ultrasonic cleaner to clean, and ultrasonic frequency is 20～50KHz, first in deionized water, cleans, and then cleans successively according to the order of acetone, absolute ethyl alcohol, deionized water, and each scavenging period is 10～15min; Then quartz substrate is taken out, after with ear washing bulb, surperficial water droplet being blown off, put into Constant Temp. Oven, 80 ℃ of design temperatures, take out after dry 20min.
The preparation of platinum alloy membrane electrode 1: prepare membrane electrode by the method for mask sputter platinum alloy in quartz substrate.
The preparation of carborundum and molybdenum disilicide composite film: adopt the mode plated film of rf magnetron sputtering, rf frequency 13.56MHz, sputtering chamber base vacuum degree 2e-4Pa～5e-3Pa, take argon gas (purity is at least 99.99%) as working gas, operating air pressure 1Pa, flow 80sccm, target spacing is 80mm, sputtering power is 200W, 500 ℃ of base reservoir temperatures when sputter, negative substrate bias 20V, first depositing silicon carbide, deposit again molybdenum disilicide, thereby obtain double membrane structure.
Anneal oxidation processing: annealing temperature is 980 ℃, annealing mixed atmosphere optimal proportion is the oxygen that the argon gas of volume fraction 70%, nitrogen that volume fraction is 20% and volume fraction are 10%, annealing time 4h.
Wherein said sputtering particle is nanoscale, and the thickness of described carborundum and molybdenum disilicide composite film is nanoscale.
A high-temperature nano Electric radiant Heating Film for double membrane structure, as shown in Figure 2, by cobalt-based alloy thin film electrode 3, quartz substrate 2, silicon carbide film layer 4, molybdenum disilicide rete 5 forms.Described quartz substrate is resistant to elevated temperatures quartz plate or quartz ampoule, or is shaped as the high temperature resistant quartz substrate of curved surface.
The preparation method of the high-temperature nano Electric radiant Heating Film of double membrane structure, its step is as follows:
Substrate is cleaned: quartz substrate utilizes ultrasonic cleaner to clean, and ultrasonic frequency is 20～50KHz, first in deionized water, cleans, and then cleans successively according to the order of acetone, absolute ethyl alcohol, deionized water, and each scavenging period is 10～15min.Then substrate is taken out, after with ear washing bulb, surperficial water droplet being blown off, put into Constant Temp. Oven, 80 ℃ of design temperatures, take out after dry 20min.
The preparation of alloy firm electrode: prepare membrane electrode by the method for mask sputter cobalt-base alloys in quartz substrate.
The preparation of carborundum and molybdenum disilicide composite film: adopt the mode plated film of rf magnetron sputtering, rf frequency 13.56MHz, sputtering chamber base vacuum degree 2e-4Pa～5e-3Pa, take argon gas (purity is at least 99.99%) as working gas, operating air pressure 1Pa, flow 80sccm, target spacing is 80mm, sputtering power is 200W, 500 ℃ of base reservoir temperatures when sputter, negative substrate bias 20V, first depositing silicon carbide, deposit again molybdenum disilicide, thereby obtain double membrane structure.
Anneal oxidation processing: annealing temperature is 980 ℃, annealing mixed atmosphere optimal proportion is the oxygen that the argon gas of volume fraction 60%, nitrogen that volume fraction is 25% and volume fraction are 15%, annealing time 4h.
Wherein said sputtering particle is nanoscale, and the thickness of described carborundum and molybdenum disilicide composite film is nanoscale.
Utilize scanning electron microscopy, X-ray diffractometer, four-point probe measurment instrument etc. that prepared laminated film in above-mentioned two embodiment is tested, analyzed, and compare with traditional Electric radiant Heating Film.On the basis of Fig. 1, Fig. 2, add voltage at substrate two ends, as shown in Figure 3, can form simple loop, can measure Electric radiant Heating Film surface temperature distribution situation.Result shows that the Electric radiant Heating Film in the present invention has clear superiority aspect high temperature, can be used in various high-temperature heat treatment occasions.
The invention discloses as mentioned above the Design & preparation method of double membrane structure high-temperature nano Electric radiant Heating Film.What enumerate here is two kinds of preferably execution modes, can do other variations roughly the same, and all employings similarity method of the present invention and similar variation thereof, all should list protection scope of the present invention in.
Claims (5)
1. a high-temperature nano Electric radiant Heating Film for double membrane structure, is made up of quartz substrate, alloy firm electrode, carborundum and molybdenum disilicide composite film; It is characterized in that: first in quartz substrate, prepare alloy firm electrode, then difference depositing silicon carbide rete and molybdenum disilicide rete in the quartz substrate that is coated with alloy firm electrode; The oxidation of molybdenum disilicide film surface is formed to thin silicon dioxide layer of protection; Wherein said sputtering particle is nanoscale, and the thickness of described carborundum and molybdenum disilicide composite film is nanoscale.
2. according to the high-temperature nano Electric radiant Heating Film of a kind of double membrane structure described in right 1, it is characterized in that: described alloy firm electrode is platinum alloy membrane electrode or cobalt-based alloy thin film electrode.
3. according to the high-temperature nano Electric radiant Heating Film of a kind of double membrane structure described in right 1, it is characterized in that: described silicon carbide film layer is the carborundum of purity 99.950%, described molybdenum disilicide rete is the molybdenum disilicide of purity 99.950%.
4. according to the high-temperature nano Electric radiant Heating Film of a kind of double membrane structure described in right 1, it is characterized in that: described quartz substrate is resistant to elevated temperatures quartz plate or quartz ampoule, or be shaped as the high temperature resistant quartz substrate of curved surface.
5. the preparation method of the high-temperature nano Electric radiant Heating Film of a kind of double membrane structure according to claim 1, it is characterized in that: utilize the method for magnetron sputtering, first mask sputter alloy firm electrode in quartz substrate, then depositing silicon carbide, deposit again molybdenum disilicide, thereby obtain double membrane structure; Concrete steps are as follows:
A) in the quartz substrate that is coated with alloy firm electrode by carborundum and molybdenum disilicide, adopt successively the mode plated film of rf magnetron sputtering; Described rf frequency is 13.56MHz; Sputtering chamber base vacuum degree is 2e-4Pa～5e-3Pa, and being at least 99.99% argon gas take purity is working gas, operating air pressure 1Pa, and flow 80sccm, target spacing is 80mm, sputtering power is 200W, 500 ℃ of quartz substrate temperature when sputter, negative substrate bias 20V;
B) under mixed atmosphere, adopt high annealing oxidation technology, by the oxidation of molybdenum disilicide film surface, form thin silicon dioxide layer of protection; Annealing temperature is 980 ℃, and annealing mixed atmosphere optimal proportion is argon gas, the nitrogen of volume fraction 15%-25% and the oxygen of volume fraction 10%-15% of volume fraction 60%-75%, annealing time 4h.
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Cited By (6)
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| CN104091882A (en) * | 2014-07-03 | 2014-10-08 | 陈国栋 | Double-layer high-radiation electrothermal film structure and manufacturing method |
| CN104144531A (en) * | 2014-08-08 | 2014-11-12 | 苏州宏久航空防热材料科技有限公司 | High heating carbon crystal plate and manufacturing method thereof |
| CN106998596A (en) * | 2017-03-02 | 2017-08-01 | 江苏森电采暖科技有限公司 | Saturated solution for preparing Electric radiant Heating Film |
| CN109536990A (en) * | 2018-10-15 | 2019-03-29 | 华南理工大学 | A kind of flat thin-film electro catalyst operation electrode and its preparation method and application |
| CN110373636A (en) * | 2019-09-02 | 2019-10-25 | 西安邮电大学 | A kind of preparation method of molybdenum silicide transistion metal compound thin-film material |
| CN112420938A (en) * | 2019-08-20 | 2021-02-26 | Tcl集团股份有限公司 | Packaging layer, photoelectric device and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104091882A (en) * | 2014-07-03 | 2014-10-08 | 陈国栋 | Double-layer high-radiation electrothermal film structure and manufacturing method |
| CN104144531A (en) * | 2014-08-08 | 2014-11-12 | 苏州宏久航空防热材料科技有限公司 | High heating carbon crystal plate and manufacturing method thereof |
| CN104144531B (en) * | 2014-08-08 | 2016-03-09 | 苏州宏久航空防热材料科技有限公司 | Brilliant plate of a kind of high heating carbon and preparation method thereof |
| CN106998596A (en) * | 2017-03-02 | 2017-08-01 | 江苏森电采暖科技有限公司 | Saturated solution for preparing Electric radiant Heating Film |
| CN106998596B (en) * | 2017-03-02 | 2019-08-30 | 江苏一森电采暖科技有限公司 | It is used to prepare the saturated solution of Electric radiant Heating Film |
| CN109536990A (en) * | 2018-10-15 | 2019-03-29 | 华南理工大学 | A kind of flat thin-film electro catalyst operation electrode and its preparation method and application |
| CN112420938A (en) * | 2019-08-20 | 2021-02-26 | Tcl集团股份有限公司 | Packaging layer, photoelectric device and preparation method thereof |
| CN110373636A (en) * | 2019-09-02 | 2019-10-25 | 西安邮电大学 | A kind of preparation method of molybdenum silicide transistion metal compound thin-film material |
| CN110373636B (en) * | 2019-09-02 | 2022-04-12 | 西安邮电大学 | Preparation method of molybdenum silicide transition metal compound film material |
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Application publication date: 20140514 |