CN102051497A - Preparation methods of gold and silver embedded target and film thereof - Google Patents
Preparation methods of gold and silver embedded target and film thereof Download PDFInfo
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- CN102051497A CN102051497A CN 201110022071 CN201110022071A CN102051497A CN 102051497 A CN102051497 A CN 102051497A CN 201110022071 CN201110022071 CN 201110022071 CN 201110022071 A CN201110022071 A CN 201110022071A CN 102051497 A CN102051497 A CN 102051497A
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Abstract
The invention relates to preparation methods of a gold and silver embedded target and a film thereof. The gold and silver embedded target contains 10-30 percent of gold and 70-90 percent of silver. When the target is prepared, a pure silver target is used for carrying out magnetron sputtering to obtain a sputtering runway, a gold slot is opened, and then gold is embedded into the gold slot by adopting a press method; and when an alloy film is prepared, gold and silver on the runway of the gold and silver embedded target are sputtered under the condition of magnetron sputtering to be mixed and deposited onto a substrate to form a gold and silver alloy film, wherein the magnetron sputtering is carried out under the conditions that the vacuum degree is 1*10<-3> to 5*10<-3>, the sputtering temperature is 20-40 DEG C, the sputtering rate is 20-200nm/minute, and the air pressure is 0.5-1Pa. In the gold and silver embedded target, gold is used for replacing partial silver on a silver target, and the gold and the silver are combined in an embedding mode, so that the utilization ratio of noble metals is high, the target cost is reduced; and the obtained target has the advantages of tight combination, high sputtering efficiency, stable property and good quality; and a prepared gold and silver alloy film has the advantages of stable property and components, higher visible light transmissivity and far infrared reflectivity than those of pure silver films, and better timeliness.
Description
Technical field
The present invention relates to a kind of use in magnetron sputtering coating target and film thereof, particularly relate to the preparation method that a kind of gold and silver is inlayed target and film thereof.
Background technology
Magnetron sputtering plating is a kind of novel physical vapor plated film mode, compares aspect a lot with the obvious advantagely with evaporation coating mode early, and it is as a proven technique comparatively, and magnetron sputtering has been applied to many fields.
Magnetron sputtering principle: between by the target utmost point (negative electrode) of sputter and anode, add a quadrature field and electric field, in high vacuum chamber, charge into needed rare gas element (being generally Ar gas), permanent magnet is formed crossed electric and magnetic field in target surfaces formation 250～350 Gausses' magnetic field with high-voltage electric field.Under effect of electric field, Ar gas is ionized into positive ion and electronics, be added with certain negative high voltage on the target, the electronics that sends from the target utmost point is increased by the effect in magnetic field and the ionization probability of working gas, form highdensity plasma body near negative electrode, the Ar ion quickens to fly to target surface under the effect of Lorentz force, with very high speed bombardment target surface, make the atom that is sputtered out on the target follow the momentum transfer principle, break away from target surface with higher kinetic energy and fly to base material deposit film forming.Magnetron sputtering generally is divided into two kinds: d.c. sputtering and radio-frequency sputtering, and the both is designed to the sputter area on the target surface run-track shaped, and wherein the dc sputtering equipment principle is simple, and when splash-proofing sputtering metal, its speed is also fast; And the use range of radio-frequency sputtering is more extensive, but except that the sputter electro-conductive material, but also sputter non-conducting material can also carry out reactive sputtering simultaneously and prepare materials such as oxide compound, nitride and carbide.If the frequency of radio frequency just becomes the microwave plasma sputter after improving, commonly used at present have a sputter of electron cyclotron resonace (ECR) type microwave plasma.
The making method of general magnetron sputtering metal coating target, comprise steps such as preparation, surface treatment, founding, hot-work and annealing, founding is ingot metal to be carried out vacuum melting by proportion of composing obtain alloy melt, and in metal mold, be shaped to when casting embryo, utilize electric-arc heating to make the alloy melt surface keep the high-temperature fusion shape synchronously, the integral surface of alloy melt is cooled off simultaneously, avoid occurring to central refrigerative situation gradually, can effectively eliminate like this and emit hole and shrinkage cavity defect by outer rim.In conjunction with above step and cooperate hot-work, annealing steps, obtain common sputtered target material.
By retrieval, application number is the manufacture method that the file of 200910008925.X discloses a kind of silver-silver-gold alloy target material, and manufacture method comprises the target raw material inserted and is heated to fusion in the smelting furnace; Molten soup after the fusion is cast; The formed ingot casting in back of will casting carries out forge hot; The idiosome that forms after the forge hot is carried out cold rolling prolonging; The cold rolling idiosome of delaying is heat-treated, to obtain the tiny silver-silver-gold alloy target material of crystal grain.This method fusion-casting process complexity, for noble metal, the utilization ratio of the target precious metal that this method makes is not high, exists simultaneously because of occurring deviation in the fusion-casting process to make the plated film sample composition uneven phenomenon occur.
Summary of the invention
The technical problem to be solved in the present invention: overcome the defective in the background technology, provide that a kind of sputtering performance is stable, colory gold and silver is inlayed target.Also providing a kind of utilizes this to inlay the method that target prepares the electrum film.
Technical scheme of the present invention
Gold and silver mosaic target equipment structure synoptic diagram of the present invention is seen Fig. 1, wherein partly represents the position that needs tight mosaic gold with oblique line, can adjust its width and size as required, reaches the purpose of each component concentration in the control film.The size of specifically inlaying part is after calculating the weight percent of Jin Yuyin according to Patterson at the formula of A, two kinds of element targets of B, area by design target runway both sides rectangle gold determines, the hit variation relation of surface composition of sputter procedure is as follows:
A
0, B
0Represent that respectively sputter begins the target surface composition of preceding two kinds of elements; Y
A, Y
BThe sputtering yield of representing two kinds of elements respectively, N
0The atomic density on expression target surface, F represents the ionic current density on target surface, t represents sputtering time.
By (1), (2) formula as can be known, along with the prolongation of sputtering time t, target surfaces A, B composition are tending towards constant respectively:
Promptly form and be tending towards constant.
The composition of A, two kinds of elements of B is respectively A in the sputtered film
s=
, B
s=
, can obtain in conjunction with (3), (4) formula again, the composition after the sputter in the alloy firm is than (A
s/ B
s) after reaching equilibrium state, have:
……………… （5）
The component proportions unanimity of target before promptly beginning with sputter.By formula (5) as can be seen, sputter under room temperature, when not considering that the target temperature raises the revaporization of alloying constituent on the alloying constituent diffusion cause and the substrate, can inlay target by the sputter gold and silver and obtain the electrum film identical, realize adjusting the purpose of thin film composition by the method that changes gold and silver ratio on the target runway with the target composition.
Gold and silver of the present invention is inlayed target, and composition is represented with weight percent, wherein golden 10%-30%, and silver-colored 70%-90%, the purity of described gold or silver is 99.99%.
The preparation method that a kind of gold and silver is inlayed target is: carry out magnetron sputtering with the fine silver target and obtain the sputter runway, inlay the composition of target determines to offer the size of golden groove and offer golden groove on silver-colored target sputter runway according to gold and silver, then silver-colored target and golden groove are cleaned, adopt method of press-fitting that gold is mounted in the golden groove.
Described golden groove is distributed in the both sides of silver-colored target sputter runway, and golden groove shape is a rectangle, long is 25-60 mm, and wide is 4-5 mm, the dimensional precision of golden groove is controlled at+0.1 mm in.
A kind of gold and silver is inlayed the method that target prepares the electrum film, comprise that base material cleans, base material is dried and the sputter coating process, wherein the sputter coating process is to make gold and silver inlay gold and silver sputter on the target runway under the magnetron sputtering condition, and mixed deposit forms the electrum film that is plated on the base material on described base material.
Described magnetron sputtering condition is: coating chamber vacuum tightness is 1 * 10
-3-5 * 10
-3Handkerchief, sputter temperature 20-40 ℃, sputter rate 20-200 nm/ minute, sputtering pressure 0.5-1 handkerchief, sputter gas are argon gas.
The thickness of described electrum film is 10-400 nm; Described base material is glass or polyethylene terephthalate.
Film thickness is controlled by the observing and controlling in early stage, mainly measures the sputter rate that satisfies target under the above sputtering condition by MCK-2B type thickness measurement and control instrument, and the selected again plated film time just can be controlled the thickness of film.
Positive beneficial effect of the present invention
(1) gold and silver of the present invention is inlayed target and is adopted part gold to substitute silver on silver-colored target, and the content of gold and silver is controlled in the specified range, adopts mosaic mode that gold and silver are combined closely, reach precious metal the utilization ratio height, reduce the purpose of target cost.
(2) gold and silver of the present invention is inlayed target does not need melting when mixing, adopt mosaic mode to carry out processing treatment, and the target combination that obtains is tight, sputtering yield height, stable performance, best in quality.
(3) gold and silver of the present invention is inlayed target and is compared with the electrum target of fusion casting, makes simply, and the gold doping amount is accurate, and thin film composition is controlled easily, has overcome fusion casting target Yin Jinyin skewness and causes the unsettled drawback of thin film composition.
(4) during electrum film preparation of the present invention, only need gold is arranged on the preparation that just can realize the electrum film on the silver-colored target sputter runway by the control sputtering condition; Need not electrum target, gold is spread all over mix the preparation of on whole silver-colored target, carrying out the electrum film as the preparation of fusion-cast method.Therefore, present method can be saved a large amount of Precious Metals-Gold.
(5) the present invention makes the sputter simultaneously of the gold and silver that are embedded on the silver-colored target runway under the magnetron sputtering condition, and mixes and be deposited on the base material, forms performance and all stable electrum film of composition.This membrane structure is evenly fine and close, and grain-size is below 100 nm, and its transmission of visible light, far infrared reflectivity all are higher than the fine silver film, and have ageing preferably.
(6) electrum method for manufacturing thin film of the present invention by factors such as control sputter temperature, pressure, power, sputter rate and coating chamber vacuum tightnesss, obtains the electrum film of compact structure, excellent property, reaches the purpose of optimizing film performance.
Description of drawings
Fig. 1 gold and silver of the present invention is inlayed the structural representation of target.The figure bend is partly represented the position of mosaic gold.
Fig. 2 gold and silver of the present invention is inlayed the left view of target.
Fig. 3 gold and silver of the present invention is inlayed the vertical view of target.
Fig. 4 electrum film of the present invention is at the microscopic appearance figure of scanning electronic microscope (SEM) lower surface.As seen from the figure, this film has careful crystal grain, and particle diameter is below 100 nm, and membrane structure is evenly fine and close.
The microscopic appearance figure of Fig. 5 electrum film of the present invention under atomic force microscope (AFM).As seen from the figure, the grain-size of this film is below 100 nm, and grain size is comparatively even, forms fine and close continuously membrane structure.
The transmission of visible light contrast of Fig. 6 electrum film of the present invention and other materials.
Curve a is a plating on glass electrum film of the present invention among the figure, and curve b is a plating fine silver film on glass, and curve c is a glass.Can find out that electrum film of the present invention has reached more than 80% in 550 its transmissivities of nm wavelength place, is higher than the transmission of visible light of fine silver film.
The far-infrared reflection spectra reflectivity contrast of Fig. 7 electrum film of the present invention and other materials.
Curve a is a plating on glass electrum film of the present invention among the figure, and curve b is a plating fine silver film on glass, and curve c is a glass.Can find out that electrum film far infrared reflectivity of the present invention is all more than 80%, than fine silver film height, farther far infrared reflectivity far above glass.
The comparison diagram of Fig. 8 fine silver film that target plates and 30 days rear surface states of placement.
Wherein a is the picture on fine silver film same day of being coated with, and b is that the fine silver film that is coated with is placed the picture after 30 days.The fine silver film is ageing relatively poor as can be seen, and 30 days rear films have become flower and lost efficacy.
The comparison diagram of Fig. 9 electrum film of the present invention and 30 days rear surface states of placement.
Wherein a is the electrum film picture on the same day, and b is the picture of electrum film placement after 30 days.Electrum film of the present invention as can be seen has ageing preferably.
Embodiment
Embodiment 1:Gold and silver is inlayed target and preparation method thereof
1. at first using purity in dustless workplace is that 99.99% silver-colored target carries out the sputter experiment in magnetic control sputtering device, accurately obtains every size of its sputter runway.The difference of sputter runway is made statistical study under sputter runway when writing down its build-up of luminance in the sputter procedure and the normal running conditions.After sputter was finished, the accurate dimension of measurements and calculations sputter runway according to the composition of the electrum film that will design, was determined the shape and the area (referring to Fig. 1, Fig. 2, Fig. 3) of slotting then on silver-colored target runway.
2. according to the composition and the fluting area of target, determine the size of flute length L, wide b.The target composition that this is routine: gold 10%, silver 90%, the purity of Jin Heyin is 99.99%; The gold groove be shaped as rectangle, long L is that 25mm, wide b are 4 mm.
3. cross-notching is accurately located on silver-colored target runway, on silver-colored target runway, run through fluting with wire cutting machine, use 120#, 240#, 600# and the meticulous polishing of 1000# sand paper cross-notching from coarse to fine then, the scale error precision of control flume is in+0.1 mm.
4. in dustless workplace, silver-colored target is cleaned degreasing, dry after clean, clean with dehydrated alcohol again, further deoil with flushing with clean water with clean-out system.
5. adopting method of press-fitting is that 99.99% gold bullion closely is mounted in the silver-colored target groove with purity, and the gold and silver of inlaying the back target material surface requires smooth, alignment.
Embodiment 2:Gold and silver is inlayed target and preparation method thereof, and is basic identical with embodiment 1, and difference is:
Target composition: gold 20%%, silver 80%; Gold flute length L is that 50mm, wide b are 4 mm.
Embodiment 3:Gold and silver is inlayed target and preparation method thereof, and is basic identical with embodiment 1, and difference is:
Target composition: gold 30%%, silver 70%; Gold flute length L is that 60mm, wide b are 5 mm.
Embodiment 4:Inlay the method that target prepares the electrum film with gold and silver
1, base material cleans: with glass is base material, and thickness of glass is 1mm, and visible light transmissivity is 93%.
(1) deoils: dip in clean gauze and get the ethanol solution wipe substrate, remove attached to dust on the base material and grease.
(2) ultrasonic cleaning: place the deionized water for ultrasonic ripple to handle twice, the contamination of further removing substrate surface base material.
(3) clean oven dry: glass is taken out,, then glass substrate is placed the loft drier dry for standby with the water wiped clean of gauze with glass surface.
2, sputter coating process
(1) charging: on the Bechtop glass substrate being installed on the substrate frame, then substrate frame is put into vacuum chamber, cover the sputtering chamber cover, check that simultaneously can substrate frame and sputtering chamber cover rotate.
(2) vacuumize: open mechanical pump, turn on the swing arm valve and begin to vacuumize, when treating that vacuum tightness reaches the 10 handkerchief left and right sides, open recirculated cooling water, open molecular pump then, continue to be evacuated to 3 * 10
-3Handkerchief.
(3) inflation and adjustment air pressure: open the argon gas switch, argon gas is fed in the vacuum chamber, regulated valve roughly is stabilized in about 0.7 handkerchief air pressure simultaneously.
(4) pre-sputter: open shielding power supply, regulate sputtering current and reach set(ting)value, gold and silver is inlayed target carried out pre-sputter 5-10 minute, stick thing, make target surface gold and silver composition be tending towards constant respectively to remove target surface; The gold and silver is here inlayed target and is the target of embodiment 2, and promptly gold is 20% in the target, silver is 80%, and golden flute length L gets 50mm, wide b gets 4 mm.
(5) sputter coating: regulate the sputtering chamber cover, make the gold and silver of the opening aligning institute sputter of cover inlay target, the rotary substrate frame begins sputter coating simultaneously.
Sputtering condition: coating chamber vacuum tightness 3 * 10
-3Handkerchief, sputter pressure are 0.7 handkerchief, and sputtering current is 0.15A, and voltage is 350V, and sputter temperature is 23 ℃, and sputter rate 30 nm/ minutes, sputtering time was 60 seconds.Concrete parameter is regulated control by CS-300 type combined magnetic-controlled sputter plated film instrument.
(6) stop sputter: after waiting to reach the sputtering time of plated film setting, close shielding power supply and stop sputter, close argon gas and vacuum pump successively, last powered-down switch and water coolant.
Coating film thickness is measured by MCK-2B type thickness measurement and control instrument, and the electrum film thickness that this example records is about 30 nm.
The surface film combination that this example obtains is good, non-oxidation phenomenon, no peeling phenomenon.Transmission of visible light (550nm) is 77.5 %, and far infrared region (4.5 μ m～25 μ m) reflectivity is 83%～86%.The electrum film that obtains is used for the making of infrared low radiation film.
Embodiment 5:Inlay the method that target prepares alloy firm with gold and silver, identical with embodiment 4 steps, difference is:
1. be substrate with glass, thickness is 1mm, and visible light transmissivity is 93%.
2. in dustless workplace, use the target of embodiment 3 to carry out film preparation by the magnetron sputtering mode, employing inlay in the target that gold is 30%, silver is 70%, golden flute length L is that 60mm, wide b are 5 mm.
3. sputtering condition: coating chamber vacuum tightness is 4 * 10
-3Handkerchief, sputter pressure are 0.7 handkerchief, and sputtering current is 0.15A, and voltage is 350V, and sputter temperature is 23 ℃, and sputter rate 30 nm/ minutes, sputtering time was 30 seconds.
The surface film combination that obtains is good, non-oxidation phenomenon, no peeling phenomenon; Transmission of visible light (550nm) is 80.3%, and far infrared region (4.5 μ m～25 μ m) reflectivity is 80%～84%, and film thickness is about 15 nm, the electrum film that obtains is used for the making of infrared low radiation film.
Embodiment 6:Inlay the method that target prepares the electrum film with gold and silver, identical with embodiment 4 steps, difference is:
1. be substrate with polyethylene terephthalate (being PET), thickness is 0.75mm, and visible light transmissivity is 91%.
2. the target that uses embodiment 1 to make by the magnetron sputtering mode in dustless workplace carries out the preparation of film, employing inlay in the target that gold is 10%, silver is 90%, golden groove shape is a rectangle, long L is that 25mm, wide b are 4 mm.
3. sputtering condition: coating chamber vacuum tightness 3 * 10
-3Handkerchief, sputter pressure are 0.5 handkerchief, and sputtering current is 0.2A, and voltage is 380V, and sputter temperature is 23 ℃, and sputter rate 50 nm/ minutes, sputtering time was 240 seconds.
The surface film combination that obtains is good, the non-oxidation phenomenon, and no peeling phenomenon, far infrared region reflectivity (4.5 μ m～25 μ m) is 89%～93%, film thickness is about 200 nm.
The electrum film that obtains is used for the making of heat reflection film.
Embodiment 7:The optical property contrast of electrum film of the present invention and fine silver film.
Under identical sputtering condition, the gold and silver of embodiment 4-6 is inlayed the film sample that film sample that target makes and fine silver target make and carry out check and analysis, and compare, referring to Fig. 6, Fig. 7 with regard to analytical results.
Fig. 6 is respectively not coated glass, fine silver silverskin and electrum film of the present invention in visible region (380～780nm) transmissivity.Fig. 7 be respectively not coated glass, fine silver silverskin and electrum film of the present invention in the far infrared region reflectivity collection of illustrative plates of (4.5～25 μ m).As can be seen, electrum film of the present invention is better than the fine silver film in the light transmission performance of visible region, and the reflecting properties in the far infrared region also is better than the fine silver film.
Embodiment 8:The Use Limitation contrast of electrum film of the present invention and fine silver film.
Keep among the embodiment 7 under identical sputtering condition gold and silver and inlay the sample that target and fine silver target are done, after clean environment normal temperature lower seal is placed 30 days, observe the surface of two kinds of samples.Sample surfaces that the fine silver target is coated with severe oxidation and peeling off can be clearly seen, continuous thin film (referring to Fig. 8) can't be formed; And the sample surfaces that the gold and silver mosaic target is coated with still is continuously and fine and close film (referring to Fig. 9).As seen the adding of gold is favourable for the oxidation-resistance of plating film sample in the target, makes the performance of film more stable, and particle is more even, and structure is fine and close more.
Claims (8)
1. a gold and silver is inlayed target, it is characterized in that: the target composition is represented with weight percent, wherein golden 10%-30%, and silver-colored 70%-90%, the purity of described gold or silver is 99.99%.
2. preparation method that the described gold and silver of claim 1 is inlayed target, it is characterized in that: carry out magnetron sputtering with the fine silver target and obtain the sputter runway, inlay the composition of target determines to offer the size of golden groove and offer golden groove on silver-colored target sputter runway according to gold and silver, then silver-colored target and golden groove are cleaned, adopt method of press-fitting that gold is mounted in the golden groove.
3. preparation method according to claim 2 is characterized in that: described golden groove is distributed in the both sides of silver-colored target sputter runway, and described golden groove shape is a rectangle, and long is 25-60 mm, and wide is 4-5 mm.
4. according to claim 2 or 3 described preparation methods, it is characterized in that: the dimensional precision of described golden groove is controlled at+0.1 mm in.
5. one kind is utilized the described gold and silver of claim 2 to inlay the method that target prepares the electrum film, comprise that base material cleans, base material is dried and the sputter coating process, it is characterized in that: described sputter coating process is to make gold and silver inlay gold and silver sputter on the target runway under the magnetron sputtering condition, and mixed deposit forms the electrum film that is plated on the base material on described base material.
6. according to the preparation method of right 5 described electrum films, it is characterized in that: described magnetron sputtering condition is: coating chamber vacuum tightness is 1 * 10
-3-5 * 10
-3Handkerchief, sputter temperature 20-40 ℃, sputter rate 20-200 nm/ minute, sputtering pressure 0.5-1 handkerchief, sputter gas are argon gas.
7. according to the preparation method of right 5 described electrum films, it is characterized in that: the thickness of described electrum film is 10-400 nm.
8. according to the preparation method of each described electrum film of right 5-7, it is characterized in that: described base material is glass or polyethylene terephthalate.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106676485A (en) * | 2017-01-04 | 2017-05-17 | 青岛蓝光晶科新材料有限公司 | Production method for runway type silicon target material |
| CN107338418A (en) * | 2017-08-30 | 2017-11-10 | 深圳先进技术研究院 | Transition metal boride metal composite target, filming equipment and application thereof |
| CN111206216A (en) * | 2020-02-27 | 2020-05-29 | 电子科技大学 | Mosaic target material experiment design method capable of controlling film components |
| CN113215431A (en) * | 2021-05-18 | 2021-08-06 | 沈阳东创贵金属材料有限公司 | White K gold target material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101805835A (en) * | 2009-02-12 | 2010-08-18 | 光洋应用材料科技股份有限公司 | Silver-gold alloy target material, manufacturing method and application thereof |
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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805835A (en) * | 2009-02-12 | 2010-08-18 | 光洋应用材料科技股份有限公司 | Silver-gold alloy target material, manufacturing method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《真空》 20000228 侯鹤岚等 溅射靶的开发与应用 37-39 1-8 , 第4期 2 * |
| 《真空科学与技术》 19870228 范玉殿 一种新型平面磁控溅射靶 42-46 1-8 第7卷, 第1期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106676485A (en) * | 2017-01-04 | 2017-05-17 | 青岛蓝光晶科新材料有限公司 | Production method for runway type silicon target material |
| CN107338418A (en) * | 2017-08-30 | 2017-11-10 | 深圳先进技术研究院 | Transition metal boride metal composite target, filming equipment and application thereof |
| CN111206216A (en) * | 2020-02-27 | 2020-05-29 | 电子科技大学 | Mosaic target material experiment design method capable of controlling film components |
| CN111206216B (en) * | 2020-02-27 | 2022-01-25 | 电子科技大学 | Mosaic target material experiment design method capable of controlling film components |
| CN113215431A (en) * | 2021-05-18 | 2021-08-06 | 沈阳东创贵金属材料有限公司 | White K gold target material and preparation method and application thereof |
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| CN102051497B (en) | 2012-11-14 |
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