CN110491772A - A kind of cleaning method of silicon base - Google Patents
A kind of cleaning method of silicon base Download PDFInfo
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- CN110491772A CN110491772A CN201910699009.9A CN201910699009A CN110491772A CN 110491772 A CN110491772 A CN 110491772A CN 201910699009 A CN201910699009 A CN 201910699009A CN 110491772 A CN110491772 A CN 110491772A
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- temperature sintering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
- B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
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Abstract
The present invention provides a kind of silicon base cleaning method, include the following steps: to obtain the silicon base for remaining carbon nanotube and other impurities, high temperature sintering processing is carried out to the silicon base；Physical cleaning is carried out to through the high temperature sintering treated silicon base；To treated that silicon base dries up through physical cleaning, reusable silicon base is then obtained.Silicon chip surface color uniformity after cleaning, immaculate, grey print problem；Secondary carbon nano tube growth basically reaches target call experiments have shown that carbon nanotube yield reaches the 91%-94% of new silicon wafer.
Description
Technical field
The invention belongs to silicon wafer cleaning process more particularly to a kind of cleaning methods of silicon base.
Background technique
In recent years, goed deep into carbon nanotube and nano materials research, the demand of carbon nanotube is increasing, wide
Application prospect also constantly show.Carbon nanotube also known as Baji-tube are that a kind of have special construction (radial dimension is
Nanometer scale, axial dimension are micron dimension, and pipe both ends are substantially all sealing) One-dimensional Quantum material.Carbon nanotube is main
Several layers to tens of layers of coaxial round tube is made of the carbon atom of hexagonal arrangement.The distance being kept fixed between layers, about
0.34nm, diameter are generally 2~20nm.And according to carbon hexagon along axial different orientation can be divided into zigzag,
Armchair and three kinds of screw type.Wherein the carbon nanotube of screw type has chiral, and zigzag and armchair carbon nanotubes
Without chirality.In general, carbon nanotube is prepared based on silicon substrate material, therefore, the cleaning quality of silicon substrate material
Have a great impact to the growth of carbon nanotube, if silicon substrate material is dealt with improperly, can may not do carbon nanotube, or manufacture
Carbon nanotube poor performance, stability and reliability are very poor.
In the prior art, it is generally received using traditional industrial standard wet clean process (RCA cleaning method) to preparing carbon
The silicon base of mitron is cleaned, and is recycled it and can be re-used for the preparation of carbon nanotube.RCA is according to alkali-strong acid-weak acid
Sequence cleaned, usually the first step be added alkaline solution be SC-1, the SC-1 solution includes H2O2And NH4OH, removal
Organic contaminations (the organic matter meeting covering part silicon chip surface, so that oxidation film and associated contamination be made to be difficult to of silicon chip surface
Removal)；Second step reinforces acid solution DHF and dissolves oxidation film；Third step adds weak acid solution to be SC-2, and the SC-2 solution includes
HCl and H2O2, removal particle, metal etc. stain, while are passivated silicon chip surface.Utilize RCA ablution, on the one hand, in carbon nanometer
In the preparation process of pipe, the oxide layer of silicon substrate surface is as the medium for promoting metallic catalyst and silicon base to combine closely, meeting
It is damaged by corrosion, is readily incorporated epitaxy defect, be unfavorable for metallic catalyst in conjunction with silicon base, and then influence the life of carbon nanotube
It is long；Another aspect this method cleaning effect is bad, is difficult the metallic catalyst for inlaying carbon nanotube root and silicon substrate surface
Residue completely remove, cause substrate recycling rate of waterused reduction.
Summary of the invention
The problem to be solved in the present invention
The purpose of the present invention is to provide a kind of cleaning methods of silicon base, it is intended to it is perishable broken to solve existing cleaning technique
The oxide layer of bad silicon substrate surface, and the problem that the carbon nanotube root residue cleaning effect to silicon substrate surface is bad.
Solution to the problem
For achieving the above object, The technical solution adopted by the invention is as follows:
A kind of cleaning method of silicon base, includes the following steps:
The silicon base for remaining carbon nanotube and other impurities is obtained, high temperature sintering processing is carried out to the silicon base；
Physical cleaning is carried out to through the high temperature sintering treated silicon base；
To treated that silicon base dries up through physical cleaning, reusable silicon base is then obtained.
Preferably, to the silicon base into the step of high temperature sintering processing, the temperature of the high temperature sintering processing is
1400~1500 DEG C, the time of the high temperature sintering processing is calcination 20~40 minutes.
Preferably, to the silicon base into the step of high temperature sintering processing, the temperature of the high temperature sintering processing is
1450 DEG C, the time of the high temperature sintering processing is calcination 30 minutes.
Preferably, to the silicon base into high temperature sintering processing the step of the following steps are included:
First high temperature sintering processing is carried out to the silicon base；To by the first high temperature sintering processing silicon base so that into
The processing of the second high temperature sintering of row.
Preferably, in the step of carrying out the processing of the first high temperature sintering to the silicon base, the first high temperature sintering processing
Temperature be 600~700 DEG C, the time of first high temperature sintering processing is 1-3 minute, what second high temperature sintering was handled
Temperature is 1400~1500 DEG C, and the time of the second high temperature sintering processing is calcination 20~40 minutes.
Preferably, in the step of carrying out the processing of the first high temperature sintering to the silicon base, the first high temperature sintering processing
Temperature be 650 DEG C, the time of first high temperature sintering processing is 2 minutes, and the temperature of the second high temperature sintering processing is
1450 DEG C, the time of the second high temperature sintering processing is calcination 30 minutes.
Preferably, it is carried out in physical cleaning step to through the high temperature sintering treated silicon base, including uses plate
Cleaning machine is cleaned.
Preferably, the time that the plate cleaning machine is cleaned is 4-6 minutes.
Preferably, to through physical cleaning, treated that silicon base carries out in drying step, the temperature of the drying is 35-45
DEG C, the wind speed of drying is 1.5-2.5m/s.
Preferably, the silicon base includes a siliceous substrate, the metallic catalyst being formed on the substrate, and edge
Carbon nanotube root in the metallic catalyst.
Invention effect
Compared with prior art, the present invention is using the method for high temperature sintering to the silicon for remaining carbon nanotube and other impurities
Substrate is handled, on the one hand, high temperature sintering, which can make the remaining carbon nanotube root of silicon base react generation with oxygen, to be waved
The carbon dioxide of hair, carbon nanotube all generates carbon dioxide volatilization after high temperature sintering；On the other hand, metal in silicon base is urged
Metal ion oxidation in agent, generates metal oxide, and metal oxide carries out high temperature sintering processing, oxidizes metal object point
Solution and fusing, the organic impurities for removing the metallic catalyst of silicon substrate surface and bringing into, while oxide layer being protected not to be destroyed, make
The carbon nanotube of loosening thoroughly falls off from silicon substrate；It is carried out at physical cleaning to through high temperature sintering treated silicon base again
Reason, physical cleaning processing mainly sufficiently remove the carbon nanotube that silicon substrate loosens, and the residual for removing chemical cleaning is miscellaneous
Matter, it is ensured that obtained silicon substrate material is without undesired impurities；Again to through physical cleaning, treated that silicon base dries up, subsequent
To reusable silicon base.The oxide layer on obtained reusable silicon substrate material surface is not damaged, is not residual
The impurity stayed.
It is suitable with new silicon wafer, after plating catalyst treatment to it, carry out the test of carbon nanotube diauxic growth, obtained carbon nanometer
Only newer silicon wafer is slightly lower for pipe yield, and carbon nano pipe array high uniformity, and spinning properties are splendid, basically reach target call.Through
It calculates, new material is lower, which has pole in terms of reducing carbon nanotube production cost compared with buying for the cleaning cost of silicon base
Big promotional value.
Meanwhile the cleaning method operating method of silicon base provided by the invention is simple, quick, cleaning effect is good, clear with original
It washes technique to compare, reduces pickling process, operation quantity is reduced, and the production cycle shortens, and realizes silicon base as carbon nanotube
The recycling of growing carrier saves carbon nanotube means of production investment, reduces carbon nanotube production cost.
Detailed description of the invention
Fig. 1 is the flow chart of cleaning silicon base provided in an embodiment of the present invention.
Fig. 2 is the effect picture of the silicon base provided by the invention cleaned using plate cleaning machine.
Fig. 3 is the effect picture of the silicon base provided by the invention cleaned by hand.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
Present example provides a kind of cleaning method of silicon base, as shown in the flow chart of Fig. 1 cleaning silicon base, including such as
Lower step:
S01. the silicon base for remaining carbon nanotube and other impurities is obtained, the silicon base is carried out at high temperature sintering
Reason；
S02. physical cleaning is carried out to through the high temperature sintering treated silicon base；
S03. to treated that silicon base dries up through physical cleaning, reusable silicon base is then obtained.
Specifically, obtaining the silicon base for remaining carbon nanotube and other impurities, carbon nanotube in above-mentioned steps S01
Root can be in mosaic texture with the metallic catalyst of silicon substrate surface, and the more difficult removal of the mosaic texture also will affect subsequent simultaneously
It uses.Specifically, the silicon base includes a siliceous substrate, the metallic catalyst being formed on the substrate, and inlay
Carbon nanotube root in the metallic catalyst.
Specifically, carrying out high temperature sintering processing to the silicon base.The method that the embodiment of the present invention first uses high temperature sintering
The silicon base of growth carbon nanotube is handled, on the one hand, high temperature sintering can make the remaining carbon nanotube root of silicon base
It is reacted with oxygen and generates volatilizable carbon dioxide, carbon nanotube all generates carbon dioxide volatilization after high temperature sintering；Another party
Face aoxidizes the metal ion in silicon base in metallic catalyst, generates metal oxide, and metal oxide carries out high temperature sintering
Processing oxidizes metal object and decomposes and melt, and the organic impurities for removing the metallic catalyst of silicon substrate surface and bringing into is protected simultaneously
Shield oxide layer is not destroyed, and the carbon nanotube loosened is made thoroughly to fall off from silicon substrate.
Preferably, to the silicon base into the step of high temperature sintering processing, the temperature of the high temperature sintering processing is
1400~1500 DEG C, the time of the high temperature sintering processing is calcination 20~40 minutes.If the temperature of high temperature sintering is excessively high, can
The oxide layer for influencing silicon substrate material and silicon base, influences secondary use, while consuming big energy, improves cost；If high temperature
The temperature of calcination is too low, then cannot reach the fusing point of metal and its oxide, not can be removed the metallic catalyst of substrate surface, nothing
Method discharges the carbon nanotube being embedded in metallic particles, the carbon nanotube loosened can not be made thoroughly to fall off from silicon substrate, shadow
Ring subsequent use.Preferably, to the silicon base into the step of high temperature sintering processing, the temperature of the high temperature sintering is 1450
DEG C, the time of the high temperature sintering is calcination 30 minutes.Calcination is carried out at this temperature, can guarantee the remaining carbon of silicon base
Nanotube root, which is more fully reacted with oxygen, generates volatilizable carbon dioxide, while can also will oxidize metal object decomposition
With fusing, the organic impurities for removing the metallic catalyst of silicon substrate surface and bringing into, while oxide layer being protected not to be destroyed, make pine
Dynamic carbon nanotube thoroughly falls off from silicon substrate.
Preferably, to the silicon base into high temperature sintering processing the step of the following steps are included:
S11. the first high temperature sintering processing is carried out to the silicon base；
S12. to the silicon base by the processing of the first high temperature sintering and then the second high temperature sintering processing of progress.
Specifically, carrying out the first high temperature sintering processing to the silicon base in above-mentioned steps S11.First high temperature sintering
Processing can make the remaining carbon nanotube root of silicon base react the volatilizable carbon dioxide of generation, high temperature sintering processing with oxygen
Carbon nanotube all generates carbon dioxide volatilization afterwards, while the metal ion in silicon base in metallic catalyst being aoxidized, and generates
Metal oxide.Preferably, in the step of carrying out the processing of the first high temperature sintering to the silicon base, at first high temperature sintering
The temperature of reason is 600~700 DEG C, and the time of the first high temperature sintering processing is 1-3 minutes.If the processing of the first high temperature sintering
Temperature is too low or calcination time is too short, then the incomplete combustion of carbon nanotube, then reacts in subsequent processing not exclusively, can not
The impurity is completely removed, will affect silicon base subsequent use；If the processing of the first high temperature sintering temperature is excessively high or the reaction time
It is too long, then under the premise of carbon nanotube pipe has burnt completely, energy loss is caused, while also increasing cost.Preferably, to institute
It states in the step of silicon base carries out the processing of the first high temperature sintering, the temperature of first high temperature sintering processing is 650 DEG C, described the
The time of one high temperature sintering processing is 2 minutes.It is handled, the carbon nanotube root of silicon base can be carried out at this temperature
Abundant calcination generates carbon dioxide, guarantees that carbon nanotube is processed clean；In addition, also can guarantee the metal onidiges in silicon base
It is oxidized generation metal oxide, is convenient for subsequent reactions.
Specifically, carrying out the second high temperature sintering to the silicon base by the processing of the first high temperature sintering in above-mentioned steps S12
Processing oxidizes metal object and decomposes and melt, the organic impurities for removing the metallic catalyst of silicon substrate surface and bringing into, release edge
Carbon nanotube in metallic particles, while oxide layer being protected not to be destroyed, make the carbon nanotube loosened from silicon substrate
Thoroughly fall off.Preferably, the described pair of silicon base by the processing of the first high temperature sintering carries out the step of the second high temperature sintering processing
In, the temperature of the second high temperature sintering processing is 1400~1500 DEG C, and the time of the second high temperature sintering processing is calcination
20~40 minutes.If the temperature of the second high temperature sintering is excessively high, the oxide layer of silicon substrate material and silicon base will affect, influence two
Secondary use, while big energy is consumed, improve cost；If the temperature of the second high temperature sintering is too low, cannot reach metal and its
The fusing point of oxide not can be removed the metallic catalyst of substrate surface, can not discharge the carbon nanotube being embedded in metallic particles,
The carbon nanotube loosened can not be made thoroughly to fall off from silicon substrate, influence subsequent use.Preferably, described pair high by first
The silicon base of warm calcination carried out in the step of the second high temperature sintering processing, and the temperature of the second high temperature sintering processing is 1450
DEG C, the time of the second high temperature sintering processing is calcination 30 minutes.The second high temperature sintering processing is carried out at this temperature, it can
Metal oxide is aoxidized completely, removes impurity, discharges the carbon nanotube being embedded in metallic particles, while protecting oxidation
Layer is not destroyed, and the carbon nanotube loosened is made thoroughly to fall off from silicon substrate.Calcination processing is carried out using two-step method, with first
The method of high temperature sintering processing handles the silicon base after growth carbon nanotube, and carbon nanotube is made all to generate carbon dioxide
Volatilization；Again using the second high temperature sintering processing method processing silicon substrate surface metal ion, oxidize metal object decompose with
Fusing, avoids under higher temperatures environment, and carbon nanotube and metal ion generate other impurities when decomposing simultaneously.
Specifically, in above-mentioned steps S02, to through the high temperature sintering, treated that silicon base carries out physical cleaning.
Preferably, it is rinsed to described by high temperature sintering processing silicon base using pure water, main purpose is
Except the impurity of silicon substrate surface.In a preferred embodiment of the invention, the pure water resistance that flushing is arranged is 12 Ω, guarantees the purity of water
High impurity is low；The washing time is 4-6 minutes, if washing time is too short, the impurity of silicon substrate surface can not be removed all,
Influence silicon substrate material subsequent use.
Preferably, after being rinsed using pure water to the silicon base, scrub process is carried out.Preferably, described in warp
High temperature sintering treated silicon base carries out in physical cleaning step, including is cleaned using plate cleaning machine.Preferably, institute
Stating the time that plate cleaning machine is cleaned is 4-6 minutes.
In an of the invention specific embodiment, the method cleaned using plate cleaning machine is as follows: by silicon wafer from
It after being taken out in the string bag, lies in a horizontal plane on the roller bearing of plate swaging machine, drives silicon wafer to move forward by roller bearing, front side of silicon wafer contact
With the brush head of roller bearing rotating Vortex, cleaning rate is 1min/ piece.As shown in Fig. 2, the silicon base cleaned using plate cleaning machine
Effect picture；As shown in figure 3, being the effect picture for the silicon base cleaned by hand；Compare the effect picture of Fig. 2 and Fig. 3 it is found that using plate
Swaging machine replaces wiping by hand, is further processed, is added during cleaning high-purity to silicon substrate surface with automation wiping device
Water constantly rinses, and drives silicon wafer to move forward by roller bearing, the brush head of front side of silicon wafer contact and roller bearing rotating Vortex, and cleaning rate is
1min/ piece removes remaining carbon and other impurity particles, and more efficient, and cleaning effect is more preferable.
Specifically, in above-mentioned steps S03, to through physical cleaning, treated that silicon base dries up, then obtaining can
The silicon base of reuse.
In a specific embodiment of the invention, the operating method of the drying are as follows: silicon base is passed through into the wiping on production line
It washes behind region and drying region is routed directly to by roller bearing, dried up the moisture adhered on silicon wafer with compressed air.
Preferably, to through physical cleaning treated silicon base dries up the step of in, the temperature of drying is 35-45
DEG C, the wind speed of drying is 1.5-2.5m/s.The oxide layer on the silicon substrate material surface ensured is not damaged, is not remaining
Impurity, it is suitable with new silicon wafer, after plating catalyst treatment to it, carry out the test of carbon nanotube diauxic growth, obtained carbon nanotube
Only newer silicon wafer is slightly lower for yield, and carbon nano pipe array high uniformity, and spinning properties are splendid, basically reach target call.Through core
It calculates, the cleaning cost of silicon base is lower compared with new material is bought, which has greatly in terms of reducing carbon nanotube production cost
Promotional value.
It is suitable with new silicon wafer, after plating catalyst treatment to it, carry out the test of carbon nanotube diauxic growth, obtained carbon nanometer
Only newer silicon wafer is slightly lower for pipe yield, and carbon nano pipe array high uniformity, and spinning properties are splendid, basically reach target call.Through
It calculates, new material is lower, which has pole in terms of reducing carbon nanotube production cost compared with buying for the cleaning cost of silicon base
Big promotional value.
Meanwhile the cleaning method operating method of silicon base provided by the invention is simple, quick, cleaning effect is good, clear with original
It washes technique to compare, reduces pickling process, operation quantity is reduced, and the production cycle shortens, and realizes silicon base as carbon nanotube
The recycling of growing carrier saves carbon nanotube means of production investment, reduces carbon nanotube production cost.
Specifically, the present invention provides following specific embodiments and is illustrated.
Embodiment 1
The 200 8 inches silicon bases for remaining carbon nanotube and other impurities are obtained, are handled using high temperature sintering.
Specifically, the silicon base after carbon Growth of Carbon Nanotubes is placed in baking oven, the temperature that high temperature sintering is arranged is 1450 DEG C, calcination
Processing 30 minutes.Physical cleaning is carried out to through the high temperature sintering treated silicon base；Flushing 4 minutes first is cleaned with pure water,
It is cleaned again with plate cleaning machine, the specific steps are silicon wafer after taking out in the string bag, is lain in a horizontal plane in plate swaging machine
On roller bearing, silicon wafer is driven to move forward by roller bearing, front side of silicon wafer contacts the brush head with roller bearing rotating Vortex, and cleaning rate is
1min/ piece.To through physical cleaning, treated that silicon base dries up, specifically, the temperature of drying is 35 DEG C, the wind speed of drying
For 2.5m/s, reusable silicon base is then obtained.
Embodiment 2:
The 200 8 inches silicon bases for remaining carbon nanotube and other impurities are obtained, at the first high temperature sintering
Reason.Specifically, the silicon base after carbon Growth of Carbon Nanotubes is placed in baking oven, the temperature of the first high temperature sintering of setting is 650
DEG C, calcination is handled 2 minutes.1500 DEG C of second high temperature sintering processing of progress, calcination are used to the silicon base through the first high temperature sintering
Processing 20 minutes.Physical cleaning is carried out to through the high temperature sintering treated silicon base；Flushing 4 minutes first is cleaned with pure water,
It is cleaned again with plate cleaning machine, the specific steps are silicon wafer after taking out in the string bag, is lain in a horizontal plane in plate swaging machine
On roller bearing, silicon wafer is driven to move forward by roller bearing, front side of silicon wafer contacts the brush head with roller bearing rotating Vortex, and cleaning rate is
1min/ piece.To through physical cleaning, treated that silicon base dries up, specifically, the temperature of drying is 40 DEG C, the wind speed of drying
For 2m/s, reusable silicon base is then obtained.
Embodiment 3:
The 200 8 inches silicon bases for remaining carbon nanotube and other impurities are obtained, at the first high temperature sintering
Reason.Specifically, the silicon base after carbon Growth of Carbon Nanotubes is placed in baking oven, the temperature of the first high temperature sintering of setting is 650
DEG C, calcination is handled 2 minutes.1400 DEG C of second high temperature sintering processing of progress, calcination are used to the silicon base through the first high temperature sintering
Processing 25 minutes.Physical cleaning is carried out to through the high temperature sintering treated silicon base；Flushing 4 minutes first is cleaned with pure water,
It is cleaned again with plate cleaning machine, the specific steps are silicon wafer after taking out in the string bag, is lain in a horizontal plane in plate swaging machine
On roller bearing, silicon wafer is driven to move forward by roller bearing, front side of silicon wafer contacts the brush head with roller bearing rotating Vortex, and cleaning rate is
1min/ piece.To through physical cleaning, treated that silicon base dries up, specifically, the temperature of drying is 45 DEG C, the wind speed of drying
For 1.5m/s, reusable silicon base is then obtained.
Comparative example 1:
RCA standard cleaning method: the silicon base after providing a carbon Growth of Carbon Nanotubes is impregnated using SPM reagent, 120 DEG C-
150 DEG C of processing silicon substrate material 10-20min, the SPM reagent are that the concentrated sulfuric acid and hydrogen peroxide 3:1 are mixed to get；Pure water is used again
It rinses, then is impregnated with APM reagent, 30~80 DEG C of 10~20min of processing silicon substrate material, the APM reagent is ammonium hydroxide: H2O2:
H2O 1:1:5 is mixed to get；Pure water rinsing is used again, then is impregnated with HPM reagent, 50~70 DEG C of processing silicon substrate materials 10~
20min, the HPM reagent are HCl:H2O2: H2O 1:1:5 is mixed to get；Pure water rinsing is used again, then is impregnated with DHF reagent,
20~25 DEG C of 10~20min of processing silicon substrate material, the hydrofluoric acid solution that the DHF reagent is 10%, then with pure water rinsing, then
Ultrasound rinsing overflow 30min is carried out, then dries up the silicon base after being cleaned.
Silicon base after cleaning that above-described embodiment 1-3 and comparative example 1 are obtained is subjected to analysis comparison.
Silicon substrate surface color after embodiment 1 is cleaned is uniform, suitable with new silicon base, carries out carbon nano tube growth examination
It tests, the results showed that reach the 90% of new silicon wafer, and carbon nano pipe array with the carbon nanotube yield of the silicon substrate bottom growth after cleaning
High uniformity, spinning properties are splendid, and target call is fully achieved.
Silicon substrate surface color after embodiment 2 is cleaned is uniform, suitable with new silicon base, carries out carbon nano tube growth examination
It tests, the results showed that reach the 94% of new silicon wafer, and carbon nano pipe array with the carbon nanotube yield of the silicon substrate bottom growth after cleaning
High uniformity, spinning properties are splendid, and target call is fully achieved.
Silicon substrate surface color after embodiment 3 is cleaned is uniform, suitable with new silicon base, carries out carbon nano tube growth examination
It tests, the results showed that reach the 91% of new silicon wafer, and carbon nano pipe array with the carbon nanotube yield of the silicon substrate bottom growth after cleaning
High uniformity, spinning properties are splendid, and target call is fully achieved.
The silicon base impurity that the cleaning of comparative example 1 obtains is remaining more, can not carry out secondary use.The cleaning method is not suitable for
Carbon nanotube industry: DHF reagent can corrode the oxide layer of silicon substrate first, silicon base be destroyed, to be unfavorable for carbon nanometer
The growth of pipe makes silicon substrate lose the value of recycling；A large amount of acid and alkaline reagent has been used in the cleaning method, has been produced
Raw liquid waste processing difficulty is big, very big to environmental disruption.Process flow is complicated, and the chemical reagent type of configuration is more, essence
Safety is not high, is unfavorable for industrial applications.RCA technique remains in silicon substrate after can not removing carbon nanotube production
Carbon.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of cleaning method of silicon base, which comprises the steps of:
The silicon base for remaining carbon nanotube and other impurities is obtained, high temperature sintering processing is carried out to the silicon base；
Physical cleaning is carried out to through the high temperature sintering treated silicon base；
To treated that silicon base dries up through physical cleaning, reusable silicon base is then obtained.
2. the cleaning method of silicon base according to claim 1, which is characterized in that the silicon base at high temperature sintering
In the step of reason, the temperature of the high temperature sintering processing is 1400~1500 DEG C, and the time of the high temperature sintering processing is calcination
20~40 minutes.
3. the cleaning method of silicon base according to claim 2, which is characterized in that the silicon base at high temperature sintering
In the step of reason, the temperature of the high temperature sintering processing is 1450 DEG C, and the time of the high temperature sintering processing is calcination 30 minutes.
4. the cleaning method of silicon base according to claim 1, the silicon base was wrapped into the step of high temperature sintering processing
Include following steps:
First high temperature sintering processing is carried out to the silicon base；To the silicon base by the processing of the first high temperature sintering and then carry out the
The processing of two high temperature sinterings.
5. the cleaning method of silicon base according to claim 4, which is characterized in that carry out the first high temperature to the silicon base
In the step of calcination is handled, the temperature of the first high temperature sintering processing is 600~700 DEG C, the first high temperature sintering processing
Time be 1-3 minute, the temperature of second high temperature sintering processing is 1400~1500 DEG C, and second high temperature sintering is handled
Time be calcination 20~40 minutes.
6. the cleaning method of silicon base according to claim 5, which is characterized in that carry out the first high temperature to the silicon base
In the step of calcination is handled, the temperature of the first high temperature sintering processing is 650 DEG C, the time of the first high temperature sintering processing
It is 2 minutes, the temperature of the second high temperature sintering processing is 1450 DEG C, and the time of the second high temperature sintering processing is calcination 30
Minute.
7. according to claim 1 in -6 any silicon base cleaning method, which is characterized in that through the high temperature sintering
Silicon base that treated carries out in physical cleaning step, including is cleaned using plate cleaning machine.
8. the cleaning method of silicon base according to claim 7, which is characterized in that the plate cleaning machine was cleaned
Time is 4-6 minutes.
9. according to claim 1 in -6 any silicon base cleaning method, which is characterized in that handle through physical cleaning
Silicon base afterwards carries out in drying step, and the temperature of the drying is 35-45 DEG C, and the wind speed of the drying is 1.5-2.5m/s.
10. according to claim 1 in -6 any silicon base cleaning method, which is characterized in that the silicon base includes
One siliceous substrate, the metallic catalyst being formed on the substrate, and the carbon nanometer being embedded in the metallic catalyst
Pipe root.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910699009.9A CN110491772B (en) | 2019-07-31 | 2019-07-31 | Cleaning method of silicon substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910699009.9A CN110491772B (en) | 2019-07-31 | 2019-07-31 | Cleaning method of silicon substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110491772A true CN110491772A (en) | 2019-11-22 |
| CN110491772B CN110491772B (en) | 2021-10-01 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1629993A (en) * | 2003-12-01 | 2005-06-22 | 富士全录株式会社 | Electrical member, electrical device, and method of manufacturing the electrical member and electrical device |
| CN101499393A (en) * | 2001-11-30 | 2009-08-05 | 索尼株式会社 | Electron emitter, cold-cathode field electron emitter, and method for manufacturing cold-cathode field electron emission display |
| US20120220106A1 (en) * | 2011-02-25 | 2012-08-30 | Tokyo Electron Limited | Carbon nanotube forming method and pre-treatment method therefor |
| CN102719888A (en) * | 2011-03-29 | 2012-10-10 | 清华大学 | A preparation method for a nanometer-microstructure substrate |
| CN104071767A (en) * | 2013-03-25 | 2014-10-01 | 苏州捷迪纳米科技有限公司 | Treating method for carbon nanotube growth substrate |
| CN109119535A (en) * | 2018-08-31 | 2019-01-01 | 京东方科技集团股份有限公司 | Flexible parent metal, flexible base board and preparation method thereof |
-
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- 2019-07-31 CN CN201910699009.9A patent/CN110491772B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101499393A (en) * | 2001-11-30 | 2009-08-05 | 索尼株式会社 | Electron emitter, cold-cathode field electron emitter, and method for manufacturing cold-cathode field electron emission display |
| CN1629993A (en) * | 2003-12-01 | 2005-06-22 | 富士全录株式会社 | Electrical member, electrical device, and method of manufacturing the electrical member and electrical device |
| US20120220106A1 (en) * | 2011-02-25 | 2012-08-30 | Tokyo Electron Limited | Carbon nanotube forming method and pre-treatment method therefor |
| CN102719888A (en) * | 2011-03-29 | 2012-10-10 | 清华大学 | A preparation method for a nanometer-microstructure substrate |
| CN104071767A (en) * | 2013-03-25 | 2014-10-01 | 苏州捷迪纳米科技有限公司 | Treating method for carbon nanotube growth substrate |
| CN109119535A (en) * | 2018-08-31 | 2019-01-01 | 京东方科技集团股份有限公司 | Flexible parent metal, flexible base board and preparation method thereof |
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