CN102839353A - Electrical arc ion plating cooling apparatus for preparing amorphous film, and applications thereof - Google Patents
Electrical arc ion plating cooling apparatus for preparing amorphous film, and applications thereof Download PDFInfo
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- CN102839353A CN102839353A CN2011101714471A CN201110171447A CN102839353A CN 102839353 A CN102839353 A CN 102839353A CN 2011101714471 A CN2011101714471 A CN 2011101714471A CN 201110171447 A CN201110171447 A CN 201110171447A CN 102839353 A CN102839353 A CN 102839353A
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Abstract
The present invention belongs to the field of film preparation, and specifically relates to an electrical arc ion plating cooling apparatus for preparing an amorphous film, and applications thereof. The cooling apparatus comprises a condensing agent input pipe, a condensing agent output pipe, a flange, an insulation washer and a sample table, wherein the flange is installed on an electrical arc ion plating furnace through the insulation washer in a sealing manner, one end of the condensing agent input pipe and one end of the condensing agent output pipe are respectively installed on the flange, penetrate through the flange, and are respectively connected with a water inlet and a water outlet of a condensing agent circulation system with controllable exterior flow rate, the other end of the condensing agent input pipe and the other end of the condensing agent output pipe are connected with the sample table, and the sample table, the part condensing agent input pipe lower than the flange, and the part condensing agent output pipe lower than the flange are positioned inside a vacuum cavity of the electrical arc ion plating furnace. The cooling apparatus of the present invention can be used for an amorphous film preparation process. In addition, the cooling apparatus of the present invention has the following characteristics that: the advantage of rapid deposition of electrical arc ion plating is provided; a substrate temperature can be effectively controlled; and purposes of film structure change and film performance increase can be achieved.
Description
Technical field
The invention belongs to the film preparation field, specifically a kind of arc ion plating refrigerating unit and application thereof that is used to prepare noncrystal membrane.
Background technology
The electric arc ion-plating deposition technology is a kind of coating technique that in a vacuum the self-holding arc discharge of cold cathode is used for evaporation source.Vacuum system feeds argon gas to 1～10
-1During Pa, between cathode targets and anode Vakuumkammer, cause arc discharge and produce the high-density metal vapor plasma, target metal positive ion deposits to the matrix surface film forming under the booster action of negative voltage electric field.This shows; The forming core of electrical arc ion plating deposition film is that mode by acceleration of ions encourages with growing up, and is received the electric field booster action by ionized target metal positive ion with the gas positive ion, constantly bombards matrix surface; The generate energy accumulation causes the matrix temperature rise.Because it is simple in structure; Sedimentation rate high (0.1～50 μ m/min); Projectile energy high (about tens ev), ionization level high (60%～80%), advantage such as diffraction property is good; Make arc ion plating (aip) obtain fast development, and become since the eighties in 20th century industrial applications one of coating technique preferably.
The performance of thin-film material is by its structures shape, and substrate temperature is the important factor that influences the deposit film weave construction in the deposition process.For example; For arc ion plating ganoine thin film (like chromium nitride, titanium nitride); The additional negative bias bombardment of the bombardment of high-energy projectile, the thermoradiation efficiency of arc light and matrix effect has all improved substrate temperature, and the CrN and the TiN that form high firmness for the deposited particles crystallization provide energy mutually.Yet,, need lower substrate temperature in the deposition process, to suppress the forming core of deposited particles in crystallisation process and to grow up if will utilize electric arc ion-plating deposition to have the thin-film material of nanocrystalline even non-crystal structure of some specified property the time.Therefore, how to suppress the accumulation of matrix energy in deposition process, become the key that solves the noncrystal membrane material prepn.
The preparation noncrystal membrane mainly utilizes magnetron sputtering technique and arc ion plating magnetic filtering technique at present.For magnetron sputtering, its principle of work be electronics under effect of electric field, in flying to the matrix process, bump with ar atmo, make argon gas ionization produce Ar
+With new electronics; New electronics flies to target surface and is fettered by magnetic field, and it has improved magnetic control target surface electronics and argon gas collision probability greatly, produces a large amount of argon ions, Ar
+Under electric field action, quicken to fly to the negative electrode target, and make target generation sputter with high-energy bombardment target surface, the neutral particle of generation sputter and target atom are deposited on and form film on the matrix.Because sedimentary neutral particle and electron energy are very low, the energy that passes to matrix is very little, and the causes substrate temperature rise is lower, helps forming the film of non-crystal structure.But, be difficult in industry, further used because there is not advantage in magnetron sputtering deposition film speed low (0.01～0.5 μ m/min) when requiring to deposit thicker noncrystal membrane.
Arc ion plating magnetic filtering technique is based on the ancillary technique of electric arc ion-plating deposition equipment; Be the transmission route of deposit film, to increase by a cover electromagnetic separation equipment (as shown in Figure 1), mainly utilize the difference of metal targets macrobead and metals ion mass-to-charge ratio that macrobead is blocked in outside the sedimentary province fully from cathode targets 1 to magnetic filter matrix 5.Owing to increased the PARTICLE TRANSPORT FROM path, making the magnetic filter matrix surface accept the projectile bombardment can sharply reduce with the target thermal radiation, thereby reaches the purpose of control matrix temperature rise, helps noncrystal membrane and deposits.The employing of magnetic filtering technique; Though eliminated oarse-grained pollution effectively; But because the loss of plasma body in transmission course; Sedimentation rate also reduces (being generally less than 2 μ m/h) significantly, and the transmission efficiency of plasma body is the highest at present also only has 25%, has caused raw-material waste and production efficiency to reduce.And it is worth noting that remove in the oarse-grained method at these, the outer magnetic straining installation of all necessary additionalamount has increased much cost.Therefore, use this technology to prepare noncrystal membrane and also be unfavorable for upward application of industry.
Summary of the invention
In order to solve magnetron sputtering technique deposit film speed low (0.01～0.5 μ m/min); When requiring to deposit thicker noncrystal membrane; The problem that is difficult in industry, use solves arc ion plating magnetic filtering technique owing to the loss of plasma body in transmission course, and sedimentation rate descends and the outer magnetic straining installation of necessary additionalamount significantly; The problem that coating cost is increased the object of the present invention is to provide a kind of arc ion plating refrigerating unit and application thereof that is used to prepare noncrystal membrane.
The objective of the invention is to realize through following technical scheme:
Refrigerating unit of the present invention comprises condensing agent input tube, condensing agent output tube, ring flange, insulating washer and sample table; Wherein ring flange is installed on the arc ion plating body of heater through the insulating washer sealing; One end of said condensing agent input tube and condensing agent output tube is installed on the ring flange respectively; And pass respectively with the entery and delivery port of the controlled condensing agent recycle system of outside flow velocity by ring flange and to be connected; The other end of condensing agent input tube and condensing agent output tube is connected with sample table, the vacuum cavity that partial condensation agent input tube below this sample table and the ring flange and condensing agent output tube all are positioned at the arc ion plating body of heater.
Wherein: said insulating washer is installed in the lower surface of ring flange, between ring flange and arc ion plating body of heater, between the lower surface of insulating washer and ring flange and insulating washer and arc ion plating body of heater, is respectively equipped with sealing-ring; Said ring flange is bolted to the body of heater reserved opening place on the arc ion plating body of heater through pottery, is connected to the negative bias lead on the ring flange, this negative bias lead through ceramic bolted on ring flange; Said sample table is the cavity of hollow, and inside is provided with dividing plate, and an end of said dividing plate is welded in the inwall of sample table upper surface, and the other end is a free end; Dividing plate is positioned at the mid-way of sample table; Between condensing agent input tube and condensing agent output tube; Divider upright is in the upper surface of sample table; Sample table is separated into two portions cavity through dividing plate, the top of two portions cavity respectively with condensing agent input tube and condensing agent output tube UNICOM, the bottom of two portions cavity communicates; Said sample table is provided with the anchor clamps of fixing base, and these anchor clamps are through being bolted on the sample table; Between said ring flange and condensing agent input tube and the condensing agent output tube, between sample table and condensing agent input tube and the condensing agent output tube and be vacuum welding between sample table and the dividing plate.
The arc ion plating refrigerating unit that the present invention is used for preparing noncrystal membrane can be used for the preparation process of noncrystal membrane; Be specially: utilize anchor clamps will treat that sedimentary matrix is fixed on the sample table; The negative bias lead of high frequency low-duty-cycle pulses bias system is anchored on the ring flange; Guarantee the electronegativity of matrix, the positive bias lead of high frequency low-duty-cycle pulses bias system is electrically connected with cathode target on being installed in arc ion plating body of heater vacuum cavity; Temperature thermocouple stretches to sample table inside by condensing agent input tube or condensing agent output tube in real time; Depositional plane is pressed close at the thermometric tip of real-time temperature thermocouple, injected condensing agent, the temperature rise of control matrix by the condensing agent input tube; Suppress the energy accumulation of matrix surface; Through real-time temperature thermocouple real-time detection and control substrate temperature, realize control deposit film structure, and then improve film performance.
Wherein: the position of said matrix is over against the cathode target, and the distance between cathode target and the matrix is 110～210mm; Said condensing agent is water or icy salt solution.
Advantage of the present invention and positively effect are:
1. refrigerating unit of the present invention; Film deposition rate and target utilization have been improved; Break through the restriction that traditional employing low deposition rate, baroque magnetron sputtering technique and arc ion plating magnetic filtering technique prepare the noncrystal membrane thinking, overcome the shortcoming of prior art.
2. refrigerating unit of the present invention is simple in structure, simple for production, with low cost, and the insulated enclosure performance is good, and temperature control in real time can feed the condensing agent of differing temps for realizing film that the deposition different performance requires, has expanded the range of application of arc ion plating.
3. refrigerating unit of the present invention can make the thin film deposition particle in transmission course, not have loss, thereby reaches the purpose that high deposition rate prepares the special construction film, has improved target utilization greatly.
4. the present invention is on the basis that guarantees sedimentation rate; Optimization design adopted high frequency (pulsed bias of 20～40kHz) low duty ratios (5～50%) (and 1000～0V) with the cooling sample table that feeds the differing temps condensing agents according to the different films of deposition; Thereby realized having suppressed the forming core in the crystallization of thin films and having grown up to carrying effective control of ability particle bombardment and energy accumulation.
5. the present invention is on the basis that guarantees film deposition rate; Feed differing temps condensing agent cooling sample table according to the different films of deposition; Realized carrying effective control of ability particle bombardment and energy accumulation; Suppress the forming core in the crystallization of thin films and grown up, realized the quick preparation brilliant film of being altogether unjustifiable, made the arc ion plating industriallization become possibility.
Description of drawings
Fig. 1 is an arc ion plating magnetic filter structural representation;
Fig. 2 looks diagrammatic cross-section for the master of refrigerating unit of the present invention;
Fig. 3 is the structural representation of refrigerating unit sample table of the present invention;
Fig. 4 is the vertical view of refrigerating unit of the present invention;
Fig. 5 is refrigerating unit application principle figure of the present invention;
Fig. 6 is the XRD result of electric arc ion-plating deposition Co alloy firm of the present invention, and wherein a curve is common electric arc ion-plating deposition methods and results, and the b curve is to adopt method of cooling result of the present invention;
Fig. 7 is the transmission electron microscope bright field image and the electron diffraction result of electric arc ion-plating deposition Co alloy firm of the present invention, and wherein a figure is common electric arc ion-plating deposition methods and results, and the b curve is to adopt method of cooling result of the present invention;
Fig. 8 is the microhardness result's of electric arc ion-plating deposition Co alloy firm of the present invention histogram, and wherein a is common electric arc ion-plating deposition methods and results, and b adopts method of cooling result of the present invention;
Wherein: 1 is the magnetic filter cathode targets, and 2 is the magnetic filter anode, and 3 is the magnetic filter pipeline, and 4 are magnetic filter guiding coil, and 5 is the magnetic filter matrix; 6 is the condensing agent input tube, and 7 is the condensing agent output tube, and 8 is scolder, and 9 is ring flange, and 10 is the flangeseal circle; 11 is insulating washer, and 12 is the furnace sealing circle, and 13 is the ring flange fixed bolt hole, and 14 is sample table, and 15 is dividing plate; 16 is bolt, and 17 is anchor clamps, and 18 is matrix, and 19 is ceramic bolt, and 20 is high frequency low-duty-cycle pulses bias system; 21 is the arc ion plating body of heater, and 22 is cathode targets, and 23 is the body of heater reserved opening, and 24 is real-time temperature thermocouple.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further:
Shown in Fig. 2～5; Refrigerating unit of the present invention comprises condensing agent input tube 6, condensing agent output tube 7, ring flange 9, insulating washer 11, sealing-ring, sample table 14 and dividing plate 15; Wherein ring flange 9 passes ring flange fixed bolt hole 13 through ceramic bolt 19 and is fixed on body of heater reserved opening 23 places on the arc ion plating body of heater 21, adopts ceramic bolt 19 to connect the insulativity that can guarantee ring flange and arc ion plating ground connection vacuum chamber; One end of said condensing agent input tube 6 is installed on the ring flange 9 and is passed with the water outlet of the controlled condensing agent recycle system of outside flow velocity by ring flange 9 and is connected, and the other end is connected with sample table 14; One end of said condensing agent output tube 7 is installed on the ring flange 9 and is passed with the water-in of the controlled condensing agent recycle system of outside flow velocity by ring flange 9 and is connected, and the other end is connected with sample table 14.This sample table 14 and the ring flange partial condensation agent input tube 6 below 9 and condensing agent output tube 7 all are positioned at the vacuum cavity of arc ion plating body of heater 21.Condensing agent input tube 6 is metal tube with condensing agent output tube 7; Being connected between ring flange 9 and condensing agent input tube 6 and the condensing agent output tube 7 adopted vacuum welding, and vacuum welding is also adopted in being connected between condensing agent input tube 6 and condensing agent output tube 7 and the sample table 14.
Said insulating washer 11 is installed in the lower surface of ring flange 9, between ring flange 9 and arc ion plating body of heater 21; Between ring flange 9 and insulating washer 11, be provided with flangeseal circle 10, between arc ion plating body of heater 21 and insulating washer 11, be provided with furnace sealing circle 12; Said ring flange 9 is through insulating washer 11 and sealing-ring and the 21 sealing installations of arc ion plating body of heater; Guarantee the insulation and the sealing of vacuum cavity in the arc ion plating body of heater 21; Thereby through sample table 14 and being connected of high frequency low-duty-cycle pulses bias system 20 applying high impulse low duty ratio negative bias for matrix 18; The negative bias lead of high frequency low-duty-cycle pulses bias system 20 is anchored on the ring flange 9 through ceramic bolt 19, guarantees the electronegativity of matrix 18 on the sample table 14.
Said sample table 14 is cavitys of a hollow, and inside is provided with dividing plate 15, and an end of this dividing plate 15 is through the inwall of vacuum welding vertical fixing in sample table 14 upper surfaces; The other end is a free end; Dividing plate 15 is positioned at the mid-way of sample table 14, and sample table 14 vertically is separated into two portions cavity, the top of two portions cavity respectively with condensing agent input tube 6 and condensing agent output tube 7 UNICOMs; The bottom of two portions cavity communicates, and this structure guarantees the abundant cooling of circulating condensing agent to hollow cavity.Described sample table 14 is provided with anchor clamps 17, and anchor clamps 17 are fixed on the surface of sample table 14 through bolt 16, and anchor clamps 17 will treat that deposit film matrix 18 is anchored on the sample table 14.
Sample table 14 is goed deep in the vacuum cavity in the arc ion plating body of heater 21 through the body of heater reserved opening 23 on the arc ion plating body of heater 21; Utilize ceramic bolt 19 that ring flange 9 is fixed in body of heater reserved opening 23 places on the arc ion plating body of heater 21, ceramic bolt 19 is anchored on the negative bias lead on the ring flange 9 simultaneously.Meanwhile, utilize flangeseal circle 10, furnace sealing circle 12 and insulating washer 11 to guarantee the sealing and the insulation of refrigerating unit and body of heater vacuum cavity.Matrix 18 is over against cathode targets 22 surfaces, and temperature thermocouple 24 stretches into sample table 14 inside through condensing agent input tube 6 in real time, and thin film deposition face is pressed close at its thermometric tip, controls its depositing temperature in real time through real-time temperature thermocouple 24.
Arc ion plating refrigerating unit of the present invention can be used for being specially in the preparation process of noncrystal membrane:
Adopt the method and the common electric arc ion electroplating method of present embodiment to compare experiment, experiment situation and result are described below:
Deposition Co alloy firm: adopt frozen water to cool off matrix at system's internal recycle as condensing agent, argon gas operating air pressure 0.2Pa, pulsed bias is-100V; Frequency is 40kHz, and dutycycle is 30%, and flame current is controlled at 40A; Target and matrix spacing 160mm obtain amorphous Co alloy firm XRD result, like b curve among Fig. 6; TEM results such as Fig. 7, b among its microhardness result such as Fig. 8.And under the same process parameter, adopt common electric arc ion electroplating method to obtain a curve among XRD result such as Fig. 6 of polycrystalline Co alloy firm, a among its microhardness result such as Fig. 8.It is 0.3～0.4 μ m/min that both sedimentation rates are.
Claims (10)
1. arc ion plating refrigerating unit that is used to prepare noncrystal membrane; It is characterized in that: comprise condensing agent input tube (6), condensing agent output tube (7), ring flange (9), insulating washer (11) and sample table (14); Wherein ring flange (9) is installed on the arc ion plating body of heater (21) through insulating washer (11) sealing; One end of said condensing agent input tube (6) and condensing agent output tube (7) is installed in respectively on the ring flange (9); And pass respectively with the entery and delivery port of the controlled condensing agent recycle system of outside flow velocity by ring flange (9) and to be connected; The other end of condensing agent input tube (6) and condensing agent output tube (7) is connected with sample table (14), the vacuum cavity that partial condensation agent input tube (6) below this sample table (14) and the ring flange (9) and condensing agent output tube (7) all are positioned at arc ion plating body of heater (21).
2. by the said arc ion plating refrigerating unit that is used to prepare noncrystal membrane of claim 1; It is characterized in that: said insulating washer (11) be installed in ring flange (9) lower surface, be positioned between ring flange (9) and the arc ion plating body of heater (21), between the lower surface of insulating washer (11) and ring flange (9) and insulating washer (11) and arc ion plating body of heater (21), be respectively equipped with sealing-ring.
3. by claim 1 or the 2 said arc ion plating refrigerating units that are used to prepare noncrystal membrane; It is characterized in that: said ring flange (9) is located through the body of heater reserved opening (23) that ceramic bolt (19) is fixed on the arc ion plating body of heater (21); Ring flange is connected to the negative bias lead on (9), and this negative bias lead is anchored on the ring flange (9) through ceramic bolt (19).
4. by the said arc ion plating refrigerating unit that is used to prepare noncrystal membrane of claim 1; It is characterized in that: said sample table (14) is the cavity of hollow; Inside is provided with dividing plate (15), and an end of said dividing plate (15) is welded in the inwall of sample table (14) upper surface, and the other end is a free end.
5. by the said arc ion plating refrigerating unit that is used to prepare noncrystal membrane of claim 4; It is characterized in that: said dividing plate (15) is positioned at the mid-way of sample table (14); Be positioned between condensing agent input tube (6) and the condensing agent output tube (7), dividing plate (15) is perpendicular to the upper surface of sample table (14), and sample table (14) is separated into two portions cavity through dividing plate (15); The top of two portions cavity respectively with condensing agent input tube (6) and condensing agent output tube (7) UNICOM, the bottom of two portions cavity communicates.
6. by the said arc ion plating refrigerating unit that is used to prepare noncrystal membrane of claim 1, it is characterized in that: said sample table (14) is provided with the anchor clamps (17) of fixing base (18), and these anchor clamps (17) are fixed on the sample table (14) through bolt (19).
7. by the said arc ion plating refrigerating unit that is used to prepare noncrystal membrane of claim 1, it is characterized in that: between said ring flange (1) and condensing agent input tube (6) and the condensing agent output tube (7), between sample table (14) and condensing agent input tube (6) and the condensing agent output tube (7) and be vacuum welding between sample table (14) and the dividing plate (15).
8. one kind by the said application that is used to prepare the arc ion plating refrigerating unit of noncrystal membrane of claim 1; It is characterized in that: it can be used in the preparation process of noncrystal membrane; Be specially: utilize anchor clamps (17) will treat that sedimentary matrix (18) is fixed on the sample table (14); The negative bias lead of high frequency low-duty-cycle pulses bias system (21) is anchored on the ring flange (9); Guarantee the electronegativity of matrix (18), the positive bias lead of high frequency low-duty-cycle pulses bias system (21) is electrically connected with cathode target (22) on being installed in arc ion plating body of heater (21) vacuum cavity; Temperature thermocouple (24) stretches to sample table (14) inside by condensing agent input tube (6) or condensing agent output tube (7) in real time; Depositional plane is pressed close at the thermometric tip of real-time temperature thermocouple (24), injected condensing agent, the temperature rise of control matrix by condensing agent input tube (6); Suppress the energy accumulation of matrix surface; Through (24) real-time detection of real-time temperature thermocouple and control substrate temperature, realize control deposit film structure, and then improve film performance.
9. by the described application of claim 8, it is characterized in that: the position of said matrix (18) is over against cathode target (22), and the distance between cathode target (22) and the matrix (18) is 110～210mm.
10. by the described application of claim 8, it is characterized in that: said condensing agent is water or icy salt solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110171447.1A CN102839353B (en) | 2011-06-23 | 2011-06-23 | Electrical arc ion plating cooling apparatus for preparing amorphous film, and applications thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110171447.1A CN102839353B (en) | 2011-06-23 | 2011-06-23 | Electrical arc ion plating cooling apparatus for preparing amorphous film, and applications thereof |
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| CN102839353A true CN102839353A (en) | 2012-12-26 |
| CN102839353B CN102839353B (en) | 2014-05-14 |
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| CN202116640U (en) * | 2011-06-23 | 2012-01-18 | 中国科学院金属研究所 | Arc ion plating cooling device for preparing amorphous thin films |
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2011
- 2011-06-23 CN CN201110171447.1A patent/CN102839353B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5171607A (en) * | 1990-01-29 | 1992-12-15 | Bausch & Lomb Incorporated | Method of depositing diamond-like carbon film onto a substrate having a low melting temperature |
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| CN2205392Y (en) * | 1994-10-26 | 1995-08-16 | 北京长城钛金技术联合开发公司 | Ion coating machine with multiple evaporation ionizing source |
| US5656091A (en) * | 1995-11-02 | 1997-08-12 | Vacuum Plating Technology Corporation | Electric arc vapor deposition apparatus and method |
| JPH09209132A (en) * | 1996-02-05 | 1997-08-12 | Nissin Electric Co Ltd | Formation of thin film and thin film forming device |
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