CN103184424A - Method for high-quality low-temperature material and processing device thereof - Google Patents
Method for high-quality low-temperature material and processing device thereof Download PDFInfo
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- CN103184424A CN103184424A CN2011104560297A CN201110456029A CN103184424A CN 103184424 A CN103184424 A CN 103184424A CN 2011104560297 A CN2011104560297 A CN 2011104560297A CN 201110456029 A CN201110456029 A CN 201110456029A CN 103184424 A CN103184424 A CN 103184424A
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- 239000000463 material Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000012530 fluid Substances 0.000 claims abstract description 57
- 238000004140 cleaning Methods 0.000 claims abstract description 40
- 238000000151 deposition Methods 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 20
- 239000010408 film Substances 0.000 claims description 16
- 239000004078 cryogenic material Substances 0.000 claims description 15
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- 238000005240 physical vapour deposition Methods 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 6
- AFYPFACVUDMOHA-UHFFFAOYSA-N chlorotrifluoromethane Chemical compound FC(F)(F)Cl AFYPFACVUDMOHA-UHFFFAOYSA-N 0.000 claims description 3
- 239000001272 nitrous oxide Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims 1
- 239000001569 carbon dioxide Substances 0.000 claims 1
- 238000000541 cathodic arc deposition Methods 0.000 claims 1
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 claims 1
- 235000019404 dichlorodifluoromethane Nutrition 0.000 claims 1
- 238000004544 sputter deposition Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 12
- 238000001953 recrystallisation Methods 0.000 abstract description 3
- 238000005469 granulation Methods 0.000 abstract 1
- 230000003179 granulation Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 230000004308 accommodation Effects 0.000 description 8
- 238000004062 sedimentation Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 230000008646 thermal stress Effects 0.000 description 5
- 235000011089 carbon dioxide Nutrition 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000427 thin-film deposition Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005530 etching Methods 0.000 description 2
- -1 methyl chlorofluoride Chemical compound 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Cleaning In General (AREA)
Abstract
A method for optimizing low-temperature material includes such steps as cleaning the material to be treated in vacuum environment, cleaning the material by supercritical fluid, constant-temp treating at 70-400 atm and 100-450 deg.C, and cleaning the material by supercritical fluid. Therefore, the constant temperature treatment is carried out under the relatively low temperature and high pressure environment, so that the material to be treated can be subjected to a process similar to fine granulation and a process similar to recrystallization, and the high-quality material with good uniformity and coverage is obtained. The invention also provides a low-temperature material quality-improving processing device.
Description
Technical field
The present invention relates to a kind of high quality method and device thereof of material, particularly relate to a kind of with method and the treatment unit thereof of cryogenic high pressure mode with the material high quality.
Background technology
In the processing processing procedure of conventional semiconductor and electronic product, major part will be passed through physical vapor deposition (PVD), arc type physical vapor deposition (PVD), or chemical vapour deposition deposition methods such as (Chemical Vaper Deposition) deposits a film at a substrate, and the pattern transfer that the little shadow gold-tinted of recycling (Lithography) and etching (Etching) technology will be desired moulding is to this substrate and pile up required three-dimensional arrangement (Architecture).
And with the made electronic product of aforesaid method, its quality major part depends on formed film quality quality in the deposition process, and the static charge of accumulating on work in-process in the processing procedure and dirty whether the removal fully.In existing processing procedure, when work in-process after finishing thin film deposition under the vacuum environment, still need vacuum breaker and move to a high temperature furnace pipe board, feed this board with the hot environment gas (Ambient gas) greater than 1000 degree Celsius again, carry out constant temperature with the work in-process that this are formed with film and handle (Anneal), so that the crystalline-granular texture of material internal can homogenizing.
But, thin-film material is under the high temperature long time treatment, have thermal stresses be accumulated in the problem in the film of producing, and thermal stresses will have the reliability of final finished and have a strong impact on, in the industry cycle under the trend to the linewidth requirements increasingly stringent, the existing technology of utilizing the long-time constant temperature of high temperature to handle to obtain high-quality thin film will be eliminated gradually, and at the soft electronic in future and bendable electronics etc. reliability be had in the electronic product of requirement for height, possibly can't continue to be employed.
In addition, existing process technique still can't propose complete and effective workaround to problem dirty and electrostatic charges accumulated in the processing procedure, this problem requires will certainly cause suitable influence to yield and the reliability of product under the trend of increasingly stringent in live width and finished product reliability.
Summary of the invention
The object of the present invention is to provide a kind of with the treatment process of relative low temperature with thin-film material Functionality, quality and appealing design materialization.
Cryogenic material high quality method of the present invention comprises one first supercutical fluid cleaning step, a constant temperature treatment step, and one second supercutical fluid cleaning step.This first supercutical fluid cleaning step is earlier a pending material to be placed a vacuum environment, with the fluid of supercritical state this pending material is cleaned afterwards again.This constant temperature treatment step be with this pending material after cleaning through this first supercutical fluid cleaning step be exposed to pressure in 70～400 normal atmosphere and temperature at Celsius 100～450 next Preset Time of environment of spending.This second supercutical fluid cleaning step is with the fluid of supercritical state this pending material through this constant temperature treatment step to be cleaned.
Preferably, in this constant temperature treatment step, be with the pending material after cleaning through this first supercutical fluid cleaning step be exposed to pressure in 200 normal atmosphere and temperature under the vacuum environments of 180 degree Celsius.
Preferably, in this constant temperature treatment step, its pressure and temperature are along with the time changes.
Preferably, this cryogenic material high quality method also comprises a deposition step between between this first supercutical fluid cleaning step and this constant temperature treatment step, and this deposition step is that the surface of the pending material after cleaning through this first supercutical fluid cleaning step forms a slice film.
Preferably, in this first supercutical fluid cleaning step and this second supercutical fluid cleaning step, this fluid is the combination that is selected from carbonic acid gas, nitrous oxide, Freon 13, methyl chlorofluoride or aforementioned substances.
Preferably, in this deposition step, be to be selected from sputter, sintering, physical vapor deposition, arc physics vapour deposition, chemical vapour deposition, or the mode of electron cyclotron resonace formula chemical vapour deposition is with the surface of this thin film deposition in this pending material.
Another object of the present invention, namely providing a kind of cryogenic material high quality treatment unit that carries out this cryogenic material high quality method that is applicable to, comprise a body, and be arranged at this intrinsic processing unit, one and be arranged at this intrinsic sedimentation unit, one and be arranged at this intrinsic supply unit, and one is arranged at this intrinsic element of fluid.Be formed with an accommodation space in this body, this processing unit is positioned at the accommodation space of this body and has a treatment chamber, and temperature and pressure in this treatment chamber can be adjusted.This sedimentation unit is positioned at the accommodation space of this body and has a deposition chambers, and a film can be plated on the surface of this pending material.This supply unit is positioned at accommodation space and this pending material of carrying of this body, makes it comply with the acquiescence flow process and carry out access in this processing unit and this sedimentation unit.This element of fluid is connected with the treatment chamber of this processing unit, and can control a fluid and import in this treatment chamber.
Beneficial effect of the present invention is: utilize and carry out the constant temperature processing under the environment of relative low temperature and relatively high pressure; make pending the material process that can be similar to subparticleization (Grain) and the process that recrystallizes (Recrystallization), to obtain uniformity coefficient (Uniformity), the good high-quality material of spreadability (Step Coverage).In addition, also can original quality is inhomogeneous, or the plated film of lower cost (Film) transforms and to change into the uniform careful fine particle high-quality thin film of quality (Thin Film) with high-quality and use in order to successive process.
Description of drawings
Fig. 1 is a schema, and first preferred embodiment of cryogenic material high quality method of the present invention is described;
Fig. 2 is a micro-real figure of photograph, this first preferred embodiment of aid illustration;
Fig. 3 is a micro-real figure of photograph, this first preferred embodiment of aid illustration;
Fig. 4 is a micro-real figure of photograph, this first preferred embodiment of aid illustration;
Fig. 5 is a schema, and second preferred embodiment of cryogenic material high quality method of the present invention is described; And
Fig. 6 is a device configuration schematic diagram, and cryogenic material high quality treatment unit of the present invention is described.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples.
Consult Fig. 1, first preferred embodiment of cryogenic material high quality method of the present invention comprises one first supercutical fluid cleaning step 1, a constant temperature treatment step 2, and one second supercutical fluid cleaning step 3.
This first supercutical fluid cleaning step 1 is earlier a pending material to be placed a vacuum environment, with the fluid of supercritical state this pending material is cleaned afterwards again.When reality is implemented, be that this pending material is statically placed in the airtight space, and with the state that is evacuated in this space, fluid is fed in this space more subsequently, after the fluid of predetermined amount to be confirmed has fed this space, namely the pressure in this space and temperature are adjusted, the target value of adjustment is the critical condition of this fluid.In the present embodiment, be as pending material with graphite, and with carbonic acid gas as this fluid, so need the temperature this space in and pressure brought up to respectively and Celsius at least 31.1 spend (℃) and 72.8 normal atmosphere (atm), certainly, also can use the fluid of other kinds, for example nitrous oxide (36.4 ℃ of critical temperatures, emergent pressure 72.5atm), Freon 13 (28.8 ℃ of critical temperatures, emergent pressure 38.7atm), methyl chlorofluoride (111.7 ℃ of critical temperatures, emergent pressure 37.4atm), the critical condition that only needs the temperature this space in and pressure to be adjusted to correspondence gets final product, and is decided by practical situation.
Utilize in this first supercutical fluid cleaning step 1 fluid-operated under the operating environment of its critical condition, so that this fluid enters above-critical state, and the fluid that is in above-critical state has high dissolving power, solubilized is built-up in dirty (contamination), the micronic dust particle (particle) on this pending thing surface, reach impurity such as static charge, and then remove the pollutent of this pending material surface effectively, make this pending material under the situation of cleaning, carry out next treatment scheme.
Continue to consult Fig. 1, in this constant temperature treatment step 2, be with this pending material after cleaning through this first supercutical fluid cleaning step 1 be exposed to pressure in 70～400atm and temperature at Celsius 100～450 next Preset Time of environment of spending.When reality is implemented, namely be that the temperature in this space and pressure condition further are promoted to 100～450 ℃ and 70～400atm Celsius respectively, in the present embodiment, be to come the constant temperature that this pending thing carried out 3 hours is handled with the operational condition of the pressure of temperature Celsius 180 ℃ and 200atm.
The constant temperature that sees through low temperature and high pressure conditions is handled; make process that this pending material can be similar to subparticleization (Grain) and recrystallize the process of (Recrystallization), and then reach the high-quality material of high uniform crystal particles degree and spreadability.
Cooperate and consult Fig. 2 to Fig. 4, Fig. 2 is real in figure for the electron microscope before handling, and Fig. 3,4 be through 3 hours 180 ℃, electron microscope after 200atm constant temperature is handled is real in figure (different enlargement ratio), by Fig. 3,4 as seen, after through 3 hours low temperature and the processing of high pressure constant temperature, the crystalline-granular texture of this pending material (graphite) changes the lattice-like that size is more consistent and arrangement is comparatively neat into by the uneven spherical shape of size before being untreated, and then make the whole uniformity coefficient of material higher, and the gap of crystal grain and intergranule also significantly dwindles, and also can significantly promote density and the whole spreadability of material.
It should be noted that, the constant temperature treatment step 2 of present embodiment is to handle with steady temperature (180 ℃) and pressure (200atm), but in fact the temperature of this constant temperature treatment step 2 and pressure also can be along with the time changes, for example, in this constant temperature step, can be earlier with 180 ℃, the operating condition of 200atm is handled the constant temperature that this pending material carried out 1.5 hours, subsequently again with 250 ℃, the operating condition of 100atm is handled the constant temperature that this pending material carried out 1 hour, at last again with 180 ℃, the operating condition of 200atm is handled the constant temperature that this pending material carried out 1 hour, so can obtain crystal grain density and the higher finished product of whole spreadability, but be noted that, above-mentioned treatment time and corresponding operating condition are used at specific pending material (being graphite in the present embodiment), then need decide on the pending material of required processing during actual enforcement, do not limited at this.
Look back Fig. 1, finish this constant temperature treatment step 2 after, namely be to carry out this second supercutical fluid cleaning step 3.In this second supercutical fluid cleaning step 3, be with the fluid of supercritical state this pending material through this constant temperature treatment step 2 to be cleaned, in the present embodiment, the mode of operation of this second supercutical fluid cleaning step 3 and condition are identical with this first supercutical fluid cleaning step 1, its effect and effect are also identical, so namely do not given unnecessary details at this.
The main purpose of first preferred embodiment of the present invention, be to carry out again high quality for the pending material product that quality is remained further improved to handle, for example, if existing pending material has passed through anneal (also may not passing through anneal as yet), but the crystal grain quality of its finished product or film formed thereon is not good, or the surface has trickle slight crack, can utilize the method for present embodiment to come the high quality processing again of this pending material secondary, obtaining density and the better crystalline-granular texture of whole spreadability, or even repair the trickle slight crack that has existed.
Consult Fig. 5, second preferred embodiment for cryogenic material high quality method of the present invention, roughly the same with first preferred embodiment, different places are, this second preferred embodiment more comprises a deposition step 4 between this first supercutical fluid cleaning step 1 and this constant temperature treatment step 2, and this deposition step 4 is that the surface of the pending material after cleaning through this first supercutical fluid cleaning step 1 forms a film.In the present embodiment, be that mode with chemical vapour deposition forms this film, but also can utilize sputter, sintering, physical vapor deposition, arc physics vapour deposition, or the mode of electron cyclotron resonace formula chemical vapour deposition is decided the surface of this thin film deposition in this pending material by the needs of reality.
The main purpose of second preferred embodiment of the present invention, mainly be to carry out high quality at the film forming material product of needs to handle, to form film by integrating this deposition step 4 with the surface at this pending material, by this constant temperature treatment step 2 this film being carried out high quality again handles, and then thin film deposition and the material high quality processing procedure of consistentization of formation, be fit to be applied in the procedure for processing of electronics or semiconductor product.
First and second preferred embodiment of cryogenic material high quality method of the present invention has the following advantages:
(1) improves quality of materials: behind the low temperature and autoclaving of this constant temperature treatment step 2, make the whole uniformity coefficient of crystalline-granular texture of pending material higher, and the gap of crystal grain and intergranule also significantly dwindles, and then can significantly promote density and the whole spreadability of material, improve the quality of material whereby.
(2) accumulation of reduction thermal stresses: the constant temperature that sees through below 450 ℃ is handled, in existing processing procedure, be higher than 1000 ℃ anneal program easily, can significantly reduce the thermal stresses accumulation of material internal, make the reliability of finished product higher, and make in the electronics and semiconductor industry that present method is more suitable for being applied to the material reliability is strict with.
Consult Fig. 6, be a kind of cryogenic material high quality treatment unit, be applicable to and carry out aforementioned cryogenic material high quality method, handle a pending material 100 is carried out high quality, this cryogenic material high quality treatment unit comprises a body 5, a processing unit 6, a sedimentation unit 7, a supply unit 8, and an element of fluid 9.
Be formed with an accommodation space 51 in this body 5, in order to the needed treatment facility of ccontaining every program, this processing unit 6 is to be arranged at this body 5 and to be positioned at this accommodation space 51, this processing unit 6 has a treatment chamber 61 that can be used for holding this pending material 100, and temperature and pressure in this treatment chamber 61 can be adjusted, in the present embodiment, pressure in this treatment chamber 61 is to adjust between 0～400atm, and temperature is to adjust in 0～450 ℃ temperature range, so that this pending material 100 is when being statically placed in this treatment chamber 61, can be exposed to aforesaid this first supercutical fluid cleaning step 1, constant temperature treatment step 2, and handle under the envrionment conditions of the second supercutical fluid cleaning step 3.
This sedimentation unit 7 is to be arranged at this body 5 and to be positioned at this accommodation space 51 and to be adjacent to this processing unit 6, this sedimentation unit 7 has the deposition chambers 71 that can hold this pending material 100, and can be film plated in the surface of this pending material 100 with one, in the present embodiment, this sedimentation unit 7 is a chemical vapor depsotition equipment, and the detailed construction of this kind equipment, configuration and effect have in the technical field under should be and know the known technology of the knowledgeable usually, namely do not give unnecessary details at this.
This supply unit 8 is to be arranged at this body 5 and to be positioned at this accommodation space 51, and can carry this pending material 100, makes this pending material 100 carry out access in this processing unit 6 and this sedimentation unit 7 according to the acquiescence flow process.In the present embodiment, but this supply unit 8 is the mechanical arm of this pending material 100 of a gripping, and this pending material 100 can be put into this treatment chamber 61 or deposition chambers 71 according to the flow process of acquiescence, or this treatment chamber 61 or the 71 interior taking-ups of this deposition chambers certainly.
This element of fluid 9 is to be arranged at this body 5 and to be connected with the treatment chamber 61 of this processing unit 6, and can control in a fluid 200 these treatment chamber 61 of input, in the present embodiment, this element of fluid 9 can be imported carbonic acid gas in this treatment chamber 61, in this treatment chamber 61, this pending material 100 is cleaned and the constant temperature processing, or carbonic acid gas extracted out in this treatment chamber 61, so that this treatment chamber 61 is in the state of vacuum.
In sum, constant temperature processing mode by cryogenic high pressure, handle pending material 100 is carried out high quality, not only can make the material after the processing can have high compactness and homogeneity, also can avoid the thermal stresses accumulation that causes at material internal because of high temperature annealing thermal treatment.
Claims (7)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104560297A CN103184424A (en) | 2011-12-30 | 2011-12-30 | Method for high-quality low-temperature material and processing device thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104560297A CN103184424A (en) | 2011-12-30 | 2011-12-30 | Method for high-quality low-temperature material and processing device thereof |
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| CN103184424A true CN103184424A (en) | 2013-07-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104867844A (en) * | 2014-02-25 | 2015-08-26 | 陈柏颖 | Material low temperature optimization method and its device |
| CN104979234A (en) * | 2014-04-08 | 2015-10-14 | 陈柏颕 | Reaction device and method thereof |
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| TW512137B (en) * | 1998-12-24 | 2002-12-01 | Tzung-Shin Liu | Low-temperature crystallization of ceramic films by high-pressure processing |
| CN1425194A (en) * | 2000-04-25 | 2003-06-18 | 东京毅力科创株式会社 | Method of depositing metal film and metal deposition cluster including supercritical drying/cleaning module |
| US20040244818A1 (en) * | 2003-05-13 | 2004-12-09 | Fury Michael A. | System and method for cleaning of workpieces using supercritical carbon dioxide |
| CN1779923A (en) * | 2005-09-23 | 2006-05-31 | 中国科学院上海技术物理研究所 | Preparation method of lead zirconate titanate ferroelectric film material which can be integrated with readout circuit |
| US20070151582A1 (en) * | 2005-12-09 | 2007-07-05 | Industrial Technology Research Institute | Supercritical fluid washing method and system |
| TW200817530A (en) * | 2006-10-12 | 2008-04-16 | Ching-Chung Lin | Method and apparatus for surface modification of film component by carbon dioxide supercritical fluid |
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2011
- 2011-12-30 CN CN2011104560297A patent/CN103184424A/en active Pending
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|---|---|---|---|---|
| TW512137B (en) * | 1998-12-24 | 2002-12-01 | Tzung-Shin Liu | Low-temperature crystallization of ceramic films by high-pressure processing |
| CN1425194A (en) * | 2000-04-25 | 2003-06-18 | 东京毅力科创株式会社 | Method of depositing metal film and metal deposition cluster including supercritical drying/cleaning module |
| US20040244818A1 (en) * | 2003-05-13 | 2004-12-09 | Fury Michael A. | System and method for cleaning of workpieces using supercritical carbon dioxide |
| CN1779923A (en) * | 2005-09-23 | 2006-05-31 | 中国科学院上海技术物理研究所 | Preparation method of lead zirconate titanate ferroelectric film material which can be integrated with readout circuit |
| US20070151582A1 (en) * | 2005-12-09 | 2007-07-05 | Industrial Technology Research Institute | Supercritical fluid washing method and system |
| TW200817530A (en) * | 2006-10-12 | 2008-04-16 | Ching-Chung Lin | Method and apparatus for surface modification of film component by carbon dioxide supercritical fluid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104867844A (en) * | 2014-02-25 | 2015-08-26 | 陈柏颖 | Material low temperature optimization method and its device |
| CN104979234A (en) * | 2014-04-08 | 2015-10-14 | 陈柏颕 | Reaction device and method thereof |
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Application publication date: 20130703 |