CN101096752A - Method for making diamond-like carbon films - Google Patents
Method for making diamond-like carbon films Download PDFInfo
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- CN101096752A CN101096752A CNA2006100867801A CN200610086780A CN101096752A CN 101096752 A CN101096752 A CN 101096752A CN A2006100867801 A CNA2006100867801 A CN A2006100867801A CN 200610086780 A CN200610086780 A CN 200610086780A CN 101096752 A CN101096752 A CN 101096752A
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Abstract
The invention discloses a making method of carbon film drilling layer grown on the base surface through sputtering and plating, which comprises the following steps: (a)providing a reacting chamber to place the base in the reacting chamber; (b)making the pressure of the reacting chamber less than 10-6torr; (c)guiding at least one gas with carbon into the reacting chamber; (d)sputtering and plating the carbon film drilling layer on the base surface of graphite target to form petal pattern. The invention has micron-size height and nanometer graded thickness, which displays good field transmitting reinforced factor.
Description
Technical field
The invention relates to a kind of making method of diamond-like carbon films, refer to that especially a kind of sputtering way of utilizing is in the grow making method of a diamond-like carbon films of substrate surface.
Background technology
Research direction for the electron emitter of present Field Emission Display, how based on the carbon material, mainly be because the short-lived and making of known metal awl electron emission assembly is difficult for, so now carbon material with chemical stability, electrical conductivity or low electron affinity that adopts as the development object more.Relevant carbon material has amorphous carbon film (amorphous carbon film), diamond film (diamond film), diamond-like carbon film (diamond-like carbon film) and CNT (carbon nano-tube) (carbon nanotube).
Because CNT (carbon nano-tube) has high depth-width ratio structure, make it have character such as low start voltage and high current emission density, promptly have good field emission enhancement factor, therefore become the field emission electron material of present hot topic.But, when CNT (carbon nano-tube) faces the successive process application,, cause the distribution of current inequality and problems such as generation minimizing in work-ing life but because of its nanoscale structures is difficult to be dispersed in the electron emission slurry of desire preparation.In addition, nanostructure is followed the big rerum natura of surface-area, will cause its factors of instability.Therefore, CNT (carbon nano-tube) need be carried out surfaction, can increase a stability of emission.
It mainly is by SP that class is bored carbon
3Three-dimensional arrangement and SP
2The amorphous carbon of two dimensional structure is formed.Because SP
3Low electron affinity and stronger mechanical properties are easily arranged, and SP
2Has preferable conduction property, so both formed classes brill carbon materials can be with characteristics such as low electron affinity and electroconductibility.
Have the advantage of low electron affinity although class is bored carbon, well-known category is bored the electron emissivity of carbon still a little less than CNT (carbon nano-tube).This major cause is that known class is bored carbon structure and do not had as the high depth-width ratio structure of CNT (carbon nano-tube).In the TaiWan, China patent No. 00444232, though mention a diamond-like carbon film, its structure is to form diamond-like carbon film on a tip as electron emission; In addition, the description in the TaiWan, China patent No. 00420723 is a mode of utilizing plasma enhanced chemical vapor deposition method (PECVD), forms diamond-like carbon film; Can find by above-mentioned two cases how well-known category brill carbon structure presents with form of film, and not have structure to be delivered so far as yet with high depth-width ratio class brill carbon.
Therefore, need a kind of making method of diamond-like carbon films at present badly.The diamond-like carbon films of this method made not only can have high depth-width ratio constitutional features, and has the characteristic of low electron affinity simultaneously, is enough to become the good electron emissive material.
Summary of the invention
The object of the present invention is to provide a kind of making method of diamond-like carbon films.
The making method of the diamond-like carbon films about sheet structure of the present invention, and this sheet structure can be arranged in the petal pattern in substrate surface.In the diamond-like carbon film that the present invention makes, the height of sheet structure is about the micron order size, and the thickness of sheet structure is about nano-grade size, so the sheet structure of diamond-like carbon film of the present invention can have high depth-width ratio feature.
For achieving the above object, the making method of diamond-like carbon films provided by the invention may further comprise the steps:
(a) provide a reaction chamber, and a substrate is inserted in this reaction chamber;
(b) make the pressure of this reaction chamber be lower than 10
-6Below the torr;
(c) import at least one carbonaceous gas in this reaction chamber; And
(d) use a graphite palladium material with sputter-deposited one diamond-like carbon films in this substrate surface;
Wherein, this diamond-like carbon film layer has sheet structure, and the sheet structure of this diamond-like carbon film layer is arranged in this substrate surface, forms a petal pattern.
Described making method, wherein this gas of being imported of step (c) also comprises rare gas element, hydrogen or its combination.
Described making method, wherein this rare gas element, this carbonaceous gas, with the importing ratio of this hydrogen be 5-20: 1-10: 0-10.
Described making method, wherein this carbonaceous gas is a hydrocarbon gas.
Described making method, wherein this hydrocarbon gas is methane or acetylene.
Described making method, wherein this rare gas element is an argon gas.
Described making method wherein before step (d) is carried out sputter, heats this substrate so that this substrate has one between 350 ℃ to 600 ℃ temperature.
Described making method wherein before step (d) is carried out sputter, heats this substrate so that this substrate has one between 400 ℃ to 550 ℃ temperature.
Described making method, wherein this substrate is semiconductor material or glass material.
Described making method, wherein the side height of this sheet structure is between 0.5 μ m to 5.0 μ m.
Described making method, wherein the side height of this sheet structure is between 0.9 μ m to 2.0 μ m.
Described making method, wherein the thickness of this sheet structure is between 0.005 μ m to 0.1 μ m.
Described making method, wherein, the thickness of this sheet structure is between 0.005 μ m to 0.05 μ m.
Described making method, wherein this sheet structure is crooked sheet structure, rectangular sheet structure or its combination.
Described making method, wherein this substrate surface also comprises a conductive layer, and this conductive layer is between this substrate and this diamond-like carbon film layer.
Described making method, wherein this conductive layer is stannic oxide, zinc oxide, zinc-tin oxide, metallic substance or alloy material.
Described making method, wherein this step (d) reaction power of carrying out this sputter is lower than below 200 watts.
Described making method, wherein this step (d) reaction power of carrying out this sputter is lower than below 150 watts.
Described making method, wherein in this step (b), the pressure of this reaction chamber is between 1 * 10
-3To 20 * 10
-3Between the torr.
In other words, the making method of diamond-like carbon films provided by the invention, its step that comprises has: a reaction chamber (a) is provided, and a substrate is inserted in the reaction chamber; (b) make the pressure of reaction chamber be lower than 10
-6Below the Torr; (c) import at least one carbonaceous gas in reaction chamber; And (d) use a graphite palladium material with sputter-deposited one diamond-like carbon films in substrate surface.Wherein, the diamond-like carbon films of the inventive method made has a sheet structure, and the sheet structure of diamond-like carbon films is arranged in a petal pattern in substrate surface.
Moreover the side height of sheet structure of the present invention can be the micron order size, preferable can be between the height of 0.5 μ m to 5.0 μ m, better can be between the height of 0.9 μ m to 2.0 μ m.And the thickness of sheet structure of the present invention can be nano-grade size, preferable can be between 0.005 μ m to 0.1 μ m, better can be between 0.005 μ m to 0.05 μ m.
Therefore, the diamond-like carbon films of the inventive method made can have high depth-width ratio feature, and has low electron affinity, to become the good electron emissive source.In addition, the present invention makes and uses radio frequency sputtering method deposition diamond-like carbon film, can realize the big area processing procedure, to reduce preparation time and cost of manufacture.
In the making method of diamond-like carbon films of the present invention, the gas alternative that step of the present invention (b) is imported also comprises hydrogen, rare gas element or its combination.Wherein, rare gas element used in the present invention can be the rare gas element that any sputter process is suitable for, and preferable argon gas or the nitrogen of can be is to provide the reaction environment of an ionized gas.Moreover the carbonaceous gas that is imported in the making method of the present invention can be any carbonaceous gas, is preferably hydrocarbon gas, and it can be methane, or acetylene etc., with carbon source as formation diamond-like carbon film of the present invention.
Spendable each gas flow is unrestricted in the invention described above sputter process, and the diamond-like carbon films structure of the demand of this gas amount of importing reaction chamber and the visual processing procedure of concentration and desire generation and adjusting.The result learns according to embodiments of the invention, and density of hydrogen is high more in the gas that imports, and formed sheet structure is thin more, and promptly density is low more; On the contrary, density of hydrogen is low more in the gas that imports, and then last formed sheet structure is just close more, and promptly density is high more.And in the inventive method, in order to the gas of the diamond-like carbon films of preparing preferable sheet structure, be preferably by rare gas element, carbonaceous gas, with the mixed gas of three kinds of gases such as hydrogen.Its ratio is with rare gas element: carbonaceous gas: hydrogen=5-20: 1-10: 0-10 is that good, better ratio is a rare gas element: carbonaceous gas: hydrogen=8-16: 4-8: 2-8.
In the making method of diamond-like carbon films of the present invention, step (d) is carried out before the sputter, and the preferable temperature that substrate can be heated to 350 ℃ to 600 ℃ earlier is to deposit a diamond-like carbon films in substrate surface.Certainly, the temperature of substrate of the present invention heating is unrestricted, preferablely can be 350 ℃ to 600 ℃, goodly can be 400 ℃ to 550 ℃.In addition, employed power is unrestricted in the sputter process of the present invention, preferablely is lower than below 200 watts, goodly is lower than below 150 watts.Moreover before carrying out sputter reaction and when also not importing gas in reaction cavity, the vacuum tightness of reaction cavity is to be controlled in 10
-5Below the torr, preferablely controlledly be formed on 10
-6Below the torr; Better person, the pressure of reaction chamber is between 1 * 10
-3To 20 * 10
-3Between the torr.
In making method of the present invention, can directly generate a diamond-like carbon films with sheet structure in substrate surface, and this sheet structure can be arranged out a petal pattern and have high depth-width ratio constitutional features in substrate surface by the sputter process of low power and low temperature.And the process parameter of sputter reaction of the present invention, for example: the vacuum tightness of temperature, sputter reaction environment, enforcement power etc., can adjust according to process requirement.
The making method of diamond-like carbon film of the present invention mainly is to feed carbonaceous gas, and dissociates carbon atom through the electricity slurry, and the diamond-like carbon film of on the substrate of heating, growing up and having sheet structure.
The sheet structure of the diamond-like carbon film of the inventive method made is unrestricted, preferable strip, the crooked sheet of can be.Wherein, the principal feature of this sheet structure is to have high depth-width ratio structure.Therefore, the diamond-like carbon film of the inventive method made can have very big field emission enhancement factor, makes it become good cathode electronics emissive source.
In making method of the present invention, the material that substrate uses is unrestricted, preferable semiconductor material or the glass material of can be.In order to increase the application of the diamond-like carbon films that the present invention makes, substrate surface alternative of the present invention also comprises a conductive layer, and conductive layer is between substrate and diamond-like carbon films.At this, but the material that above-mentioned conductive layer was suitable for can be any electro-conductive material, preferable stannic oxide, zinc oxide, zinc-tin oxide, metallic substance or the alloy material of can be.
In one preferred embodiment, the substrate that the inventive method is used is during as the glass material, and this glass baseplate surface is to be coated with a conductive layer, so that the diamond-like carbon films of sheet structure is formed at conductive layer surface.So, can be provided the diamond-like carbon films of a voltage in sheet structure by conductive layer, the diamond-like carbon films that the present invention is made can be used as electron emission and uses.
In another preferred embodiment, the substrate that the inventive method is suitable for is the semiconductor material, because baseplate material has the property of conducting, so the diamond-like carbon films of sheet structure is directly to be formed at substrate surface, promptly becomes an electron emission source.
Compared to known CNT (carbon nano-tube) material, the growth process temperatures that the class of micron order structure used in the present invention is bored carbon material is lower, and can be directly grown in substrate surface, so help the application of processing procedure.In addition, the sheet structure that class of the present invention is bored carbon has high depth-width ratio feature, so can have very high field emission enhancement factor, to be applicable to the Application Areas of various electron emission, for example: the cold cathode emissive source of an emitting module, Field Emission Display or planar light source etc.
Description of drawings
The synoptic diagram of the sputter that Fig. 1 uses when making diamond-like carbon films for a preferred embodiment of the present invention.
Fig. 2 a is scanning type electron microscope (SEM) the photo figure that the surface of a preferred embodiment of the present invention making has the substrate front side of diamond-like carbon films.
Fig. 2 b is scanning type electron microscope (SEM) the photo figure that the surface of a preferred embodiment of the present invention making has the substrate side surfaces of diamond-like carbon films.
Fig. 2 c is the diamond-like carbon films that a preferred embodiment of the present invention is made, and it is scraping scanning type electron microscope (SEM) the photo figure that places substrate front side.
Fig. 3 is Raman (Raman) spectrogram of the diamond-like carbon films of embodiment two to embodiment six mades.
Embodiment
Following content will illustrate the making method of the diamond-like carbon films of the present invention's one preferred embodiment, please in the lump with reference to shown in Figure 1.Fig. 1 makes the synoptic diagram of the employed sputter 100 of diamond-like carbon films for present embodiment.
At first, provide a reaction chamber 100 in order to sputter, and this reaction chamber 100 comprises a well heater 10 in order to heated substrates 1, a plummer 11 in order to bearing substrate 1, one in order to the power supply device 13 of bestowing target 12 voltages and a plurality ofly provide unit A, B, C in order to the gas that reactant gases is provided.Note that when the present invention makes diamond-like carbon films that gas provides the unit to set up according to the gas condition of process requirement or to reduce, be not limited to the described equipment of present embodiment.
Then, clean substrate 1 surface, and it is inserted on the plummer 11 of reaction chamber 100, with fixing base 1.Wherein, the substrate 1 that present embodiment adopted is the silicon wafer of semiconductor material.Utilize a vacuum extractor 14 that reaction chamber 100 is evacuated to 1 * 10
-5Below the torr, and utilize well heater 10 that substrate 1 is heated to 400 ℃.
Then, provide unit A, B, C to provide reaction required gas, and utilize mass flow control device (mass flow controller, figure does not show) to control the flow that each gas enters this reaction chamber 100 by gas.Wherein, present embodiment gas provides unit A, B, C to be respectively a gas supply source that argon gas, methane, hydrogen is provided.And present embodiment is whether to import reaction chamber 100 by each gas supply valve a1, b1, c1 and by process conditions to control three kinds of gases.Wherein, the gas that present embodiment imports reaction chamber 100 includes argon gas, methane and hydrogen, and its gas ratio is 2: 1: 1.
In this example, after reactant gases imported reaction chamber 100, the pressure in the reaction chamber was controlled at 9 * 10 approximately
-3Torr.Certainly, the environmental stress of sputter reaction of the present invention is not the described content of limit present embodiment, can adjust according to process requirement.
Immediately, with the 200W radio frequency power graphite target 12 is carried out 30 minutes pre-sputter (pre-sputtered) reaction after, to remove the pollutent that target 12 surfaces may exist.Then, open masking shield 111, and 70 minutes sputter reaction is carried out on substrate 1 surface, with the diamond-like carbon films of growing up in substrate 1 surface.
Please refer to shown in Fig. 2 a, Fig. 2 b and Fig. 2 c, Fig. 2 a is scanning type electron microscope (SEM) the photo figure that surface that present embodiment is made has the substrate front side of diamond-like carbon films, and Fig. 2 b is scanning type electron microscope (SEM) the photo figure that surface that present embodiment is made has the substrate side surfaces of diamond-like carbon films.Fig. 2 c is the diamond-like carbon films that present embodiment is made, and scrapes scanning type electron microscope (SEM) the photo figure that places substrate front side.
Shown in Fig. 2 a and Fig. 2 b, the diamond-like carbon films of present embodiment made is crooked sheet or rectangular sheet structure, and these sheet structures are arranged out a spatial petal pattern in substrate 1 surface.Wherein, the center line average of the sheet structure of present embodiment is about 1 μ m, and the mean thickness of each sheet structure is about between the 10nm to 20nm, and forms the structure of the height " depth-width ratio " that the present invention advocated.In addition, shown in Fig. 2 c, the diamond-like carbon films that will grow up to, scrape place substrate after, the diamond-like carbon films mean thickness of this moment is between 10nm to 20nm, its width then can be between 1～3 μ m.
Therefore, the diamond-like carbon films of present embodiment made has high depth-width ratio constitutional features, and the employed substrate of present embodiment is to be a conductive semiconductor material, so can directly apply to the purposes of electron emission source.
The table 1 different gas ratio among the row embodiment 2 to embodiment 6 of will knowing clearly.
Table 1
| Argon gas | Methane | Hydrogen | |
| Embodiment two | 8 | 8 | 8 |
| Embodiment three | 10 | 5 | 5 |
| Embodiment four | 10 | 5 | 2 |
| Embodiment five | 16 | 8 | 0 |
| Embodiment six | 16 | 4 | 0 |
Fig. 3 is Raman (Raman) spectrogram of the diamond-like carbon films of embodiment two to embodiment six mades.By learning among Fig. 3, the diamond-like carbon film series of strata of made of the present invention are by SP
3Three-dimensional arrangement and SP
2Two dimensional structure is formed, and therefore having one is about 1332cm
-1The absorption peak and of tetrahedron diamond structures be about 1580cm
-1The absorption peak of plane stone ink structure.
In sum, the inventive method can be made a class with micron-stage sheet-like structure and be bored carbon, because this micron-stage sheet-like structure has the feature of high depth-width ratio, so can become the good electron emissive material, to be applied to the cold cathode emissive source of an emitting module, Field Emission Display or planar light source etc.
The foregoing description is only given an example for convenience of description, and the interest field that the present invention advocated should be as the criterion so that claim is described certainly, but not only limits to the foregoing description.
Claims (19)
1, a kind of making method of diamond-like carbon films may further comprise the steps:
(a) provide a reaction chamber, and a substrate is inserted in this reaction chamber;
(b) make the pressure of this reaction chamber be lower than 10
-6Below the torr;
(c) import at least one carbonaceous gas in this reaction chamber; And
(d) use a graphite palladium material with sputter-deposited one diamond-like carbon films in this substrate surface;
Wherein, this diamond-like carbon film layer has sheet structure, and the sheet structure of this diamond-like carbon film layer is arranged in this substrate surface, forms a petal pattern.
2, making method as claimed in claim 1, wherein this gas of being imported of step (c) also comprises rare gas element, hydrogen or its combination.
3, making method as claimed in claim 2, wherein this rare gas element, this carbonaceous gas, with the importing ratio of this hydrogen be 5-20: 1-10: 0-10.
4, making method as claimed in claim 1, wherein this carbonaceous gas is a hydrocarbon gas.
5, making method as claimed in claim 4, wherein this hydrocarbon gas is methane or acetylene.
6, making method as claimed in claim 2, wherein this rare gas element is an argon gas.
7, making method as claimed in claim 1 wherein before step (d) is carried out sputter, heats this substrate so that this substrate has one between 350 ℃ to 600 ℃ temperature.
8, making method as claimed in claim 1 wherein before step (d) is carried out sputter, heats this substrate so that this substrate has one between 400 ℃ to 550 ℃ temperature.
9, making method as claimed in claim 1, wherein this substrate is semiconductor material or glass material.
10, making method as claimed in claim 1, wherein the side height of this sheet structure is between 0.5 μ m to 5.0 μ m.
11, making method as claimed in claim 1, wherein the side height of this sheet structure is between 0.9 μ m to 2.0 μ m.
12, making method as claimed in claim 1, wherein the thickness of this sheet structure is between 0.005 μ m to 0.1 μ m.
13, making method as claimed in claim 1, wherein, the thickness of this sheet structure is between 0.005 μ m to 0.05 μ m.
14, making method as claimed in claim 1, wherein this sheet structure is crooked sheet structure, rectangular sheet structure or its combination.
15, making method as claimed in claim 1, wherein this substrate surface also comprises a conductive layer, and this conductive layer is between this substrate and this diamond-like carbon film layer.
16, making method as claimed in claim 15, wherein this conductive layer is stannic oxide, zinc oxide, zinc-tin oxide, metallic substance or alloy material.
17, making method as claimed in claim 1, wherein this step (d) reaction power of carrying out this sputter is lower than below 200 watts.
18, making method as claimed in claim 1, wherein this step (d) reaction power of carrying out this sputter is lower than below 150 watts.
19, making method as claimed in claim 1, wherein in this step (b), the pressure of this reaction chamber is between 1 * 10
-3To 20 * 10
-3Between the torr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100867801A CN101096752A (en) | 2006-06-26 | 2006-06-26 | Method for making diamond-like carbon films |
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|---|---|---|---|
| CNA2006100867801A CN101096752A (en) | 2006-06-26 | 2006-06-26 | Method for making diamond-like carbon films |
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|---|---|
| CN101096752A true CN101096752A (en) | 2008-01-02 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102214722A (en) * | 2011-04-18 | 2011-10-12 | 中国石油大学(华东) | Palladium-doped carbon film/oxide/semiconductor material with photoconductive effect |
| CN104513969A (en) * | 2013-09-27 | 2015-04-15 | 群创光电股份有限公司 | Structure with diamond-like carbon, fingerprint identifier and production method of fingerprint identifier |
| US9516759B2 (en) | 2013-09-27 | 2016-12-06 | Innolux Corporation | Multilayer structure, fingerprint identification device and manufacturing method thereof |
-
2006
- 2006-06-26 CN CNA2006100867801A patent/CN101096752A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102214722A (en) * | 2011-04-18 | 2011-10-12 | 中国石油大学(华东) | Palladium-doped carbon film/oxide/semiconductor material with photoconductive effect |
| CN104513969A (en) * | 2013-09-27 | 2015-04-15 | 群创光电股份有限公司 | Structure with diamond-like carbon, fingerprint identifier and production method of fingerprint identifier |
| US9516759B2 (en) | 2013-09-27 | 2016-12-06 | Innolux Corporation | Multilayer structure, fingerprint identification device and manufacturing method thereof |
| CN104513969B (en) * | 2013-09-27 | 2017-06-06 | 群创光电股份有限公司 | Structure, fingerprint identifier and its manufacture method with quasi cobalt carbon diaphragm |
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Open date: 20080102 |