CN101492811B - Self-air-suction vacuum plating method - Google Patents
Self-air-suction vacuum plating method Download PDFInfo
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- CN101492811B CN101492811B CN2009100583894A CN200910058389A CN101492811B CN 101492811 B CN101492811 B CN 101492811B CN 2009100583894 A CN2009100583894 A CN 2009100583894A CN 200910058389 A CN200910058389 A CN 200910058389A CN 101492811 B CN101492811 B CN 101492811B
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Abstract
The invention discloses a self suction vacuum coating method. In the method, a gas suction hood is arranged between a substrate and an evaporation source or a sputtering target, a membrane is deposited in advance when the vacuum degree does not meet the preset value before formal membrane deposition, then deposition is stopped and vacuumizing is continued. After the air pressure is rapidly decreased to the preset value by making use of the self suction action of the membrane, the formal membrane deposition is carried out. The method greatly shortens the period of vacuum suction, reduces active gas composition in the residual gas, increases the purity of the membrane, and is applicable to preparing active metal or alloy membrane thereof by using physical vapor deposition method. The method has the characteristics of simple operation and strong universality without changing the original coating equipment.
Description
Technical field
The present invention relates to the physical gas phase deposition technology field of film, be specifically related to a kind of self-air-suction vacuum plating method.
Background technology
The physical vapor deposition of film comprises methods such as evaporation, sputter, ion plating, ion beam assisted depositing, the bundle plating of ionization group; These nearly all methods all need be carried out under high vacuum even UHV condition; To improve the purity of film; Reduce the pollution of entrap bubble, particularly oxygen in the Vakuumkammer, water vapour isoreactivity gas to film.But, vacuumize time with labor, seriously restricting the production efficiency of thin-film material and device.
Utilizing the air-breathing principle of material to vacuumize is a kind of method of extensive employing; Like titanium sublimation pump and sputter ion pump; They belong to ultrahigh vacuum pump, and its ultimate principle is evaporation or the fresh titanium film of sputter one deck in Vakuumkammer, reacting generating compounds such as residual oxygen, nitrogen in titanium film and the Vakuumkammer; Thereby consume these gas, realize the function that vacuumizes.These pumps have versatility, but cost an arm and a leg, and getter material is consumptive, need periodic replacement, and common high vacuum coating system is not equipped with.
Except that the aspirator pump of above-mentioned two kinds of versatilities, a large amount of special getter device and method have been reported in the patent documentation.As:
USP 6468043B1 discloses a kind of method of utilizing getter material to vacuumize; Tie up to the metal and the alloy firm thereof such as inwall sputtered titanium, zirconium, hafnium, vanadium, scandium of a suction muffler; Return to atmospheric condition then, remove sputtering target after, this chamber and a vacuum system are coupled together; Through these getter films of heat activation, to obtain ultrahigh vacuum(HHV).
One group of USP 6589599B1,6858254B2; 20030207030A1 and 20050072356A1 disclose a kind of getter device that is easy to load and unload and method that reduces the Vakuumkammer internal contamination and the time of bleeding; System utilizes sample transfer means that getter device is put into substrate position; After air-breathing, it is removed, move into the method for substrate again.
Chinese patent 200580008280.x discloses the method that absorbs the oxygen G&W during a kind of vacuum deposition of sulfide films; Tie up to the deposition sulfide before or between depositional stage, evaporate one or more air-breathing materials simultaneously, this air-breathing material and sulfide are not same material.
The drawback of these getter devices is:
(1) the getter device structure is special; Exhausted be placed on internal vacuum chamber mostly, be equivalent to built-in aspirator pump, require and Vakuumkammer in physical dimension, the aspect such as be electrically connected and mate and can use; Therefore transplantability is poor, and the against vacuum system does not have versatility.
(2) in the use of getter material, have limitation, getter material and Coating Materials are cut leave, promptly two kinds of materials are inequality, consider to utilize the activity of Coating Materials self to carry out air-breathing.
Problem to be solved by this invention is: how a kind of self-air-suction vacuum plating method is provided; When preparation reactive metal or alloy firm; Can overcome existing defective in the prior art, utilize the getter action of himself to come gas clean-up, reduce the film pollution.
Technical problem proposed by the invention is to solve like this: a kind of self-air-suction vacuum plating method is provided; It is the alloy firm that the preparation reactive metal perhaps contains reactive metal on the substrate in being in Vakuumkammer; Used device comprises Vakuumkammer, substrate, evaporation source or sputtering target, vacuum pump; It is characterized in that, at first between substrate and evaporation source or sputtering target, be provided with an air-suction cover, operate according to following steps then: a, Vakuumkammer is evacuated to preset pressure values P1; B, under the substrate shielding status, deposit the layer of active metal in advance or contain the alloy firm of reactive metal; C, stop thin film deposition, continue to be evacuated to preset pressure values P2, P2＜P1; D, make substrate be in no shielding status, the reactive metal that formally deposition is identical with step (b) material on substrate perhaps contains the alloy firm of reactive metal.
According to self-air-suction vacuum plating method provided by the present invention; It is characterized in that; Said reactive metal comprises magnesium, aluminium, calcium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, rubidium, strontium, yttrium, zirconium, niobium, palladium, barium, hafnium, tantalum, lead and rare earth metal, and the said alloy firm that contains reactive metal is the alloy material that contains one or more above-mentioned reactive metals.
According to self-air-suction vacuum plating method provided by the present invention, it is characterized in that air-suction cover adopts stainless steel or aluminium, copper, titanium and alloy thereof to process.
According to self-air-suction vacuum plating method provided by the present invention, it is characterized in that, adopt baffle plate or station rotating mechanism in step (b), to make substrate be in shielding status.
According to self-air-suction vacuum plating method provided by the present invention, it is characterized in that making substrate be in device used under the shielding status in the step (2) is the substrate means for screening, said substrate means for screening comprises baffle plate or station rotating mechanism.
According to self-air-suction vacuum plating method provided by the present invention, it is characterized in that this method is used for evaporation coating method or sputter coating method or ion plating method or ion beam assisted depositing method or ionization group bundle plating method.
Beneficial effect of the present invention: sedimentary in advance film is equivalent to one deck sacrifice layer, and this step can't too much consume Coating Materials.Because itself just there are passivation layers such as one deck oxide compound on reactive metal and alloy raw material surface, in the sputter coating flow process of routine, adopt the method for preparatory sputter to remove these impurity usually, need to sacrifice the thin-film material of initial sputter equally.In the sputter coating flow process of routine, be after vacuum tightness reaches requirement only, at first carry out preparatory sputter, carry out formal sputter then at once.And essence of the present invention is when vacuum tightness does not also reach requirement, at first carries out pre-deposition, utilizes the getter action of this layer expendable material to bleed, treat that vacuum tightness is reduced to required value after, carry out formal sputter or evaporation again.
The present invention is based on the improvement on the coating operation flow process, need not do a bit change to film coating apparatus, on any physical vapor deposition device, all can use, and it is extensive on equipment, to have flexibility, the characteristics of highly versatile.Very strong universality is also arranged on Coating Materials, be applicable to all reactive metals and alloy thereof.This method can be quickened the process that vacuumizes greatly, particularly can reduce the dividing potential drop of vacuum indoor oxygen, water vapour isoreactivity gas effectively, improves the purity of film.
Fig. 1 is a vacuum vapor plating system architecture synoptic diagram;
Fig. 2 is a sputter coating system architecture synoptic diagram;
Fig. 3 is the many targets sputter coating system architecture synoptic diagram with station wheelwork;
Fig. 4 is the sputter coating system architecture synoptic diagram of band air-suction cover;
Fig. 5 self-air-suction vacuum plating process flow diagram of the present invention;
Fig. 6 is the contrast by the X ray diffracting spectrum of the ytterbium film of the ytterbium film of the present invention's preparation and common process preparation.
Wherein, 1 is Vakuumkammer; 2 is substrate; 3 is film; 4 is vaporize; 5 is crucible; 6 is crucible heater; 7 is baffle plate; 8 is substrate heater; 9 is sputtering target; 10 are the station rotation; 11 is air-suction cover.
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
Fig. 5 is a self-air-suction vacuum plating process flow diagram of the present invention, and shown operation steps (1) as follows is evacuated to preset value P1 with Vakuumkammer; (2) under the substrate shielding status, deposit thin film in advance; (3) stop thin film deposition, continue to be evacuated to preset value P2, P2＜P1; (4) make substrate be in no shielding status, formally deposit film on substrate.This method is used for evaporation coating method or sputter coating method or ion plating method or ion beam assisted depositing method or ionization group bundle plating method.Be applicable to that reactive metal perhaps contains the alloy firm of reactive metal, comprises magnesium, aluminium, calcium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, rubidium, strontium, yttrium, zirconium, niobium, palladium, barium, hafnium, tantalum, lead, rare earth metal and alloy thereof.
Adopt self-air-suction vacuum plating technical process of the present invention, can on like Fig. 1, Fig. 2, conventional PVD filming equipment shown in Figure 3, realize.
As shown in Figure 1, be the structural representation of vacuum vapor plating system, used device comprises Vakuumkammer 1, substrate 2; Vaporize 4, crucible 5, crucible heater 6, baffle plate 7; Substrate heater 8, following in conjunction with concrete operations step of the present invention: as after vacuum reaches P1, to make the vaporize 4 in the crucible 5 receive thermal evaporation to feeding heating current in the crucible heater 6; This moment baffle plate 7 be in closing condition, evaporate thin film in advance after, close well heater 6; Continue to vacuumize reach P2 after, open baffle plate 7 substrate 2 exposed, carry out formal evaporation.
Fig. 3 is the many targets sputter coating system architecture synoptic diagram with station wheelwork, and wherein 9a, 9b, 9c and 9d are sputtering targets, and 2 is substrate, and 10 is the station rotating mechanism.Have at least 1 to be reactive metal or alloys target in the sputtering target, suppose to be positioned at the 9a position.Following in conjunction with concrete operations step of the present invention: at first be evacuated to P1, feed argon gas sputter thin film in advance then, this moment, substrate 2 was positioned at the position of the opposite 9c of target 9a, so can not deposit upper film on the substrate 2.Stop sputter subsequently, close argon gas, continue to be evacuated to P2, utilize station rotating mechanism 10 that substrate 2 is turned to the position of target 9a, make substrate 2, feed argon gas and carry out formal sputtering in the face of target 9a.
Embodiment 1: adopt sputter equipment shown in Figure 2 to carry out ytterbium depositing of thin film (used device comprises Vakuumkammer 1, substrate 2, baffle plate 7 and sputtering target 9).Ytterbium is a kind of lanthanide rare metal, and it is Yb that chemistry meets, and has piezoresistive effect, is used to prepare the ytterbium pressure transmitter.Adopt flow process sputter ytterbium film as shown in Figure 5: when vacuum tightness reaches 2 * 10
-3During Pa, feed the high-purity argon gas of about 1Pa, began preparatory sputter ytterbium film 15 minutes, sputtering current is 0.4A, the about 280V of sputtering voltage.This moment, baffle plate 7 was closed, so the ytterbium film is to be deposited on baffle plate bottom surface and the vacuum chamber inwall, and can not be deposited on the substrate 2.After stopping preparatory sputter, close argon gas, continue to vacuumize, because the getter action of deposition ytterbium film in the cavity, after about 30 minutes, the vacuum tightness in the chamber is reduced to 7.0 * 10 very soon
-4Pa.Feed argon gas this moment, carries out formal sputter.Carried out sputter in advance once more preceding 5 minutes of formal sputtering, opened baffle plate 7 subsequently and make substrate 2, the ytterbium film has been sputtered on the substrate in the face of ytterbium target 9.Compare with the technical process of routine, if vacuum tightness reaches 2 * 10
-3Behind the Pa, not preparatory sputter ytterbium film, but use molecular pump to vacuumize fully, needed about 2 hours 40 minutes can reach 7.0 * 10
-4The vacuum tightness of Pa.Adopt of the present inventionly to vacuumize, can practice thrift over half bleeding the time from gettering.
Embodiment 2: adopt the sputter equipment of band air-suction cover shown in Figure 4 to carry out the ytterbium depositing of thin film.The step of plated film and experimental technique condition are identical with embodiment 1, when vacuum tightness reaches 2 * 10
-3During Pa, feed the preparatory sputter of argon gas 15 minutes, sputtering current is 0.4A, the about 280V of sputtering voltage.Stop to close argon gas after the preparatory sputter and continue to vacuumize, because air-suction cover 11 has increased air-breathing area effectively, after about 20 minutes, the vacuum tightness in the chamber is reduced to 7.0 * 10
-4Pa.Compare with the embodiment that does not have air-suction cover 1, can further shorten the time that vacuumizes.
Fig. 6 is the contrast of the present invention from the X ray diffracting spectrum of the ytterbium film of air-breathing technology and common process preparation, and the time of totally bleeding of the two all is about 2 hours, but base vacuum is different, has reached 7.0 * 10 from gettering
-4Pa, and hanging down of common process is 1.0 * 10
-3Pa.Can find out obviously that from the contrast of the two XRD figure spectrum the ytterbium film of common process preparation also has the diffraction peak of ytterbium oxide except the diffraction peak of ytterbium, show that the ytterbium film of this prepared exists tangible oxidation.This oxidation is not the oxidation on surface behind the ytterbium film taking-up Vakuumkammer.Because although surface oxidation is inevitable, this zone of oxidation is very thin, is difficult to detect with common X-ray diffraction method.Therefore, oxidation is intravital oxidation, the oxidation that promptly in the film preparation process, takes place.And review the ytterbium film of the present invention from air-breathing prepared, just there is not tangible oxidation peak.
Claims (5)
1. self-air-suction vacuum plating method; It is the alloy firm that the preparation reactive metal perhaps contains reactive metal on the substrate in being in Vakuumkammer; Used device comprises Vakuumkammer, substrate, evaporation source or sputtering target, vacuum pump; It is characterized in that, at first between substrate and evaporation source or sputtering target, be provided with an air-suction cover, operate according to following steps then: a, Vakuumkammer is evacuated to preset pressure values P1; B, under the substrate shielding status, deposit the layer of active metal in advance or contain the alloy firm of reactive metal; C, stop thin film deposition, continue to be evacuated to preset pressure values P2, P2＜P1; D, make substrate be in no shielding status, the formal reactive metal that deposition is identical with step b material on substrate perhaps contains the alloy firm of reactive metal.
2. self-air-suction vacuum plating method according to claim 1; It is characterized in that; Said reactive metal is magnesium, aluminium, calcium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, rubidium, strontium, yttrium, zirconium, niobium, palladium, barium, hafnium, tantalum, lead and rare earth metal, and the said alloy firm that contains reactive metal is the alloy material that contains one or more above-mentioned reactive metals.
3. according to claim 1 or 2 said self-air-suction vacuum plating methods, it is characterized in that air-suction cover employing stainless steel or aluminium or copper or titanium or titanium alloy are processed.
4. self-air-suction vacuum plating method according to claim 1 and 2 is characterized in that, adopts baffle plate or station rotating mechanism in step b, to make substrate be in shielding status.
5. self-air-suction vacuum plating method according to claim 1 and 2 is characterized in that, this method is used for evaporation coating method or sputter coating method or ion plating method or ion beam assisted depositing method or ionization group bundle plating method.
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| CN101492811B true CN101492811B (en) | 2012-01-25 |
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| WO2021199479A1 (en) * | 2020-04-01 | 2021-10-07 | キヤノンアネルバ株式会社 | Film formation device, device for controlling film formation device, and film formation method |
| CN112626460A (en) * | 2020-11-23 | 2021-04-09 | 上海晶维材料科技有限公司 | High-performance Ti-Co-RE target material and preparation method of high-suction-capacity film getter |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1447368A (en) * | 2003-02-14 | 2003-10-08 | 厦门火炬福大显示技术有限公司 | Omni range evapo transpiration type suction unit |
| CN1561405A (en) * | 2001-09-27 | 2005-01-05 | 纳幕尔杜邦公司 | Dual-source, single-chamber method and apparatus for sputter deposition |
| CN101100739A (en) * | 2007-08-02 | 2008-01-09 | 哈尔滨工业大学 | Method for preparing thin film by using magnetron sputtering |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1561405A (en) * | 2001-09-27 | 2005-01-05 | 纳幕尔杜邦公司 | Dual-source, single-chamber method and apparatus for sputter deposition |
| CN1447368A (en) * | 2003-02-14 | 2003-10-08 | 厦门火炬福大显示技术有限公司 | Omni range evapo transpiration type suction unit |
| CN101100739A (en) * | 2007-08-02 | 2008-01-09 | 哈尔滨工业大学 | Method for preparing thin film by using magnetron sputtering |
Non-Patent Citations (4)
| Title |
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| . |
| 说明书第1页第2段1－2行 |
| 说明书第2页具体实施方式3－4行. |
| 说明书第2页第5段5－7行 |
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