CN103628026A - Chrome-doped crystalline tungsten film and preparation method thereof - Google Patents
Chrome-doped crystalline tungsten film and preparation method thereof Download PDFInfo
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- CN103628026A CN103628026A CN201310627059.9A CN201310627059A CN103628026A CN 103628026 A CN103628026 A CN 103628026A CN 201310627059 A CN201310627059 A CN 201310627059A CN 103628026 A CN103628026 A CN 103628026A
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Abstract
The invention discloses a chrome-doped crystalline tungsten film and a preparation method thereof. The chrome-doped crystalline tungsten film is prepared through direct and continuous sputtering by utilizing magnetron sputtering equipment, and subsequent annealing treatment is omitted. The preparation method specifically comprises the steps of putting a tungsten target on a direct current sputtering stage in a magnetron sputtering equipment vacuum chamber, putting a chrome target in a sputtering area of the tungsten target, and putting a substrate on a sample stage; vacuumizing the vacuum chamber until the back bottom is vacuum, filling argon into the vacuum chamber, adjusting the argon flow and the sputtering pressure, and adjusting the sputtering direct current and the no load ratio; after pre-sputtering for a period of time before deposition sputtering, adjusting the substrate to the sputtering area, and preparing the chrome-doped crystalline tungsten film in the set sputtering deposition time. The process is simple to operate, and the film is crystalline and does not fall off. The chrome-doped crystalline tungsten film obtained through magnetron sputtering dispenses with the subsequent heat treatment process.
Description
Technical field
The present invention relates to a kind of tungsten material for hydrogen helium irradiation, more particularly, refer to a kind of chromium-doped crystalline state W film and preparation method thereof.
Background technology
Magnetron sputtering is a kind of widely used physical gas-phase deposite method, and its advantage is high at film deposition rate, and operating air pressure is lower, is conducive to continuous discharge.Magnetron sputtering technique key point is, in sputter equipment, introduce magnetic field, reduced on the one hand the gaseous tension of reaction process, simultaneously, under the conditions such as same electric current, gas, magnetron sputtering technique can significantly improve efficiency and the sedimentation rate of sputter on the other hand.Magnetron sputtering technique, can be little to substrate bombardment effect near the of target and its by plasma containment as a modern technique.Can reduce substrate damage and reduce depositing temperature, be favourable for the deposition of some films, but at pre-deposition or when cleaning target, and it is very necessary keeping the bombardment effect of appropriate ion pair substrate.In magnetron sputtering technique, very high for the requirement of target, need to carry out for target coolingly, and need to carry out pre-sputtering for target, reach the object of cleaning removal of impurities.Underlayer temperature, sputtering power and cavity air pressure are all the important parameters that affects thin film deposition.(P.J.Kblly, R.D.Anlell.Magnetron sputtering:a review of recent developments and applications.Vacuum, 2000,56:159-172) processing unit of magnetically controlled DC sputtering technology is simple, has higher sedimentation rate in deposition process.On metal coating, there is certain advantage especially, can plate micron-sized thickness, for the research of metal alloy provides the special best method of preparing sample.Going deep into of nucleosynthesis Industrial materials research in recent years, requires to have the performance characteristic that tungsten sill qualified and various metals doping is convenient to material under Study of Hydrogen, helium plasma irradiation to change, and is badly in need of processing method simple and easy to do, easy to prepare.Because chromium metal block material has the characteristic hindering to internal migration to hydrogen atom, to be badly in need of chromium-doped tungsten sill and to be convenient to research, magnetron sputtering plating provides may.Because major part plating is film formed, be noncrystalline membrane, also will carry out anneal, may cause film oxidation and come off, to research, brought certain difficulty.
The people such as V.Kh.Alimov that have that prepare tungsten based film material of report utilize sputtering sedimentation to plate the tungsten film of thickness >=0.4 μ m in the world at present, because film is non-crystalline state, must carry out anneal and be converted into crystalline state film and could study, easily like this cause coming off of oxidation and film.（V.Kh.Alimov,J.Roth,W.M.Shu,D.A.Komarov，K.Isober，T.Yamanishi.,Deuterium?trapping?in?tungsten?deposition?layers?formed?by?deuterium?plasma?sputtering.Journal?of?Nuclear?Materials,2010,399:225-230）。V.
deng people, utilize magnetron sputtering into about the thick non-crystalline state tungsten film of 10 μ m, if also need to carry out crystallization processing for the irradiation effect of Study of Hydrogen helium, in crystallization and thermal treatment process, because minimal thickness is excessive, be easy to come off, and due to inner tensions, also may cause the phenomenons such as film fracture to occur.（V.
，B.Zajec,D.Dellasega,M.Passoni.,Hydrogen?permeation?through?disordered?nanostructure?tungsten?films.Journal?of?Nuclear?Materials,2012,429:92-98）。
Summary of the invention
The object of the invention is to propose a kind of chromium-doped crystalline state W film and preparation method thereof, through the inventive method, prepare chromium-doped crystalline state W film without carrying out heat treated, concrete steps are to be that tungsten target material is placed on the d.c. sputtering platform in magnetic control sputtering device vacuum chamber, chromium target is placed on to the maximum sputtering zone of tungsten target, cleaned substrate is placed in the sample table in vacuum chamber; Vacuum chamber is evacuated to back end vacuum, to vacuum chamber, is filled with argon gas, and regulate argon flow amount and sputter to press, and then regulate No Load Ratio and sputter galvanic current; Before deposition sputter, pre-sputtering, after for some time, regulates substrate to sputter area, and the default sputtering sedimentation time starts to prepare chromium-doped crystalline state W film.This technological operation is simple, and film is crystalline state, does not come off, and the chromium-doped crystalline state W film making saves heat treatment process.
The present invention is a kind of method that adopts magnetron sputtering technique to prepare chromium-doped crystalline state W film, and the method includes the following step:
Step 1: the clean of tungsten substrate
The mass percent purity of tungsten substrate is 99.999%;
First tungsten substrate is placed in to deionized water and carries out ultrasonic cleaning 2～5 minutes, be placed in again alcohol and carry out ultrasonic cleaning 2～5 minutes, be placed in again acetone and carry out ultrasonic cleaning 2～5 minutes, be placed in again deionized water and carry out ultrasonic cleaning 2～5 minutes, be placed in again alcohol and carry out ultrasonic cleaning 2～5 minutes, take out, after seasoning, obtain clean rear tungsten substrate.The set of frequency of ultrasonic cleaning is 30KHz.
Step 2: the placement of target and substrate
First tungsten target material is placed on the d.c. sputtering platform in magnetic control sputtering device vacuum chamber, then chromium target is placed on to the maximum sputtering zone of tungsten target;
Tungsten substrate after step 1 is cleaned is placed in the sample table in vacuum chamber;
The mass percent purity of tungsten target material is 99.99%, and the mass percent purity of chromium target is 99.99%.
Step 3: regulate sputtering pressure, sputter direct current
After the operation of step 2 is completed, close vacuum chamber, vacuum chamber is evacuated to back end vacuum 4 * 10
-4～5.5 * 10
-4pa;
Then, to vacuum chamber, be filled with argon gas, and to regulate argon flow amount and sputtering pressure, argon flow amount be 19～21scc, sputtering pressure is 0.7～0.9Pa; The volume percent purity of argon gas is 99.999%;
Then, regulate No Load Ratio 50 and sputter galvanic current 0.14～0.16A;
Step 4: magnetron sputtering made membrane
The splash-proofing sputtering process parameter setting according to step 3, opens run switch, after pre-sputtering 5～10min, regulates substrate to sputter area, and then, after magnetron sputtering deposition time 5～8h, closing device, takes out chromium-doped crystalline state W film.
Advantage of the present invention:
1. technique is simple, and easy handling is tested controlledly, and doped element chromium can be by regulating target quantity to control chromium content.
2. chromium-doped W film is crystalline state, saves film thermal treating processes, and film does not come off.
3. starting material are easily purchased, and cost is low, only need one-time continuous sputtering sedimentation.
Accompanying drawing explanation
Fig. 1 is substrate and footwear material schematic diagram staggered relatively in magnetron sputtering equipment.
Figure 1A is a kind of modes of emplacement schematic diagram of target on target platform.
Figure 1B is the another kind of modes of emplacement schematic diagram of target on target platform.
Fig. 2 is the XRD figure spectrum that adopts the chromium-doped crystalline state W film that the inventive method makes in embodiment 1.
Fig. 3 adopts the chromium-doped crystalline state W film that the inventive method makes to amplify the stereoscan photograph of 1000 times in embodiment 1.
Fig. 4 adopts the chromium-doped crystalline state W film that the inventive method makes to amplify the stereoscan photograph of 5000 times in embodiment 1.
Fig. 5 is the profile scanning electromicroscopic photograph that adopts the chromium-doped crystalline state W film that the inventive method makes in embodiment 1.
Fig. 6 is the chromium content energy spectrogram that adopts the chromium-doped crystalline state W film that the inventive method makes in embodiment 1.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The present invention prepares chromium-doped crystalline state W film with magnetic control sputtering device and has solved the preparation problem of tungsten sill in fusion research.Experimental implementation is simple, does not need too much complicated equipment, and starting material are easily purchased, and only needs one-time continuous deposition.Film is crystalline state, saves heat treatment process, and film does not come off, and can directly carry out experimental study use.The thin-film material of preparation is chromium-doped crystalline state W film by XRD analysis, and peak value in [110], [200], [211], [220] overlap completely with tungsten base peak.
Chromium-doped crystalline state W film prepared by the present invention is 2.5 microns～3.5 microns through scanning electron microscopic observation thickness.
Chromium-doped crystalline state W film prepared by the present invention, the content of its chromium is 2.0wt%～13.8wt%.
The present invention is a kind of method that adopts magnetron sputtering technique to prepare chromium-doped crystalline state W film, and the method includes the following step:
Step 1: the clean of tungsten substrate
The mass percent purity of tungsten substrate is 99.999%;
First tungsten substrate is placed in to deionized water and carries out ultrasonic cleaning 2～5 minutes, be placed in again alcohol (mass percent concentration is 70%) and carry out ultrasonic cleaning 2～5 minutes, be placed in again acetone (mass percent concentration is 99.5%) and carry out ultrasonic cleaning 2～5 minutes, be placed in again deionized water and carry out ultrasonic cleaning 2～5 minutes, be placed in again alcohol and carry out ultrasonic cleaning 2～5 minutes, take out, after seasoning, obtain clean rear tungsten substrate.The set of frequency of ultrasonic cleaning is 30KHz.
Step 2: the placement of target and substrate
First tungsten target material is placed on the d.c. sputtering platform in magnetic control sputtering device vacuum chamber, then chromium target is placed on to the maximum sputtering zone of tungsten target;
Tungsten substrate after step 1 is cleaned is placed in the sample table in vacuum chamber;
In the present invention, in order to guarantee the doping of chromium, chromium target can cut into the bulk of 4 * 4 * 2mm specification, and the mode that chromium target is placed on tungsten target material is placed for symmetrical.General chromium target is selected 2,4 or 6 numbers of blocks.
The mass percent purity of tungsten target material is 99.999%, and the mass percent purity of chromium target is 99.999%.
Step 3: regulate sputtering pressure, sputter direct current
After the operation of step 2 is completed, close vacuum chamber, vacuum chamber is evacuated to back end vacuum 4 * 10
-4～5.5 * 10
-4pa;
Then, to vacuum chamber, be filled with argon gas, and to regulate argon flow amount and sputtering pressure, argon flow amount be 19～21scc, sputtering pressure is 0.7～0.9Pa; The volume percent purity of argon gas is 99.999%;
Then, regulate No Load Ratio 50 and sputter galvanic current 0.14～0.16A;
Step 4: magnetron sputtering made membrane
The splash-proofing sputtering process parameter setting according to step 3, opens run switch, after pre-sputtering 5～10min, regulates substrate to sputter area, and then, after magnetron sputtering deposition time 5～8h, closing device, takes out chromium-doped crystalline state W film.
Shown in Fig. 1, in figure, numbering refers to respectively radio frequency platform 1, vacuum chamber 2, argon inlet mouth 3, vacuum extractor 4, sample table 5 and sample autobiography platform 6.
The mass percent purity of tungsten target material is 99.999%, and the mass percent purity of tungsten substrate is 99.999%, and the mass percent purity of chromium target is 99.999%.
The pre-treatment of tungsten substrate: first tungsten substrate is placed in to deionized water and carries out ultrasonic cleaning 3 minutes, be placed in again alcohol (mass percent concentration is 70%) and carry out ultrasonic cleaning 3 minutes, be placed in again acetone (mass percent concentration is 99.5%) and carry out ultrasonic cleaning 2 minutes, be placed in again deionized water and carry out ultrasonic cleaning 5 minutes, be placed in again alcohol and carry out ultrasonic cleaning 5 minutes, take out, after seasoning, obtain clean rear tungsten substrate.The set of frequency of ultrasonic cleaning is 30KHz.
Close vacuum chamber, vacuum chamber 2 is vacuumized, make vacuum tightness in vacuum chamber 2 reach the back end vacuum values 5 * 10 of sputtering instrument
-4during Pa, to vacuum chamber 2, be filled with argon gas (volume percent purity is 99.999%), argon flow amount is 20scc, and vacuum sputtering is pressed and is transferred to 0.8Pa; Adjusting sputter galvanic current is that 0.16A and dutycycle are 50.
Before deposition sputter, the first pre-sputtering of tungsten target 10 minutes, then regulates tungsten substrate in sample table 5 to the sputter area of radio frequency platform 1, and it is 5h that deposition sputtering time is set.
After sputter, closing device, takes out sample and carries out Performance Detection.
The sample that embodiment 1 is made adopts X-ray diffractometer to carry out material phase analysis to the chromium-doped W film of preparation, as shown in Figure 2, the film that preparation is described has been crystalline film, its peak value in [110], [200], [211], [220] overlap completely with tungsten base peak.
The sample that embodiment 1 is made is at electronic scanning electricity Microscopic observation, and film surface is smooth, as shown in Figure 3 and Figure 4; Film has been done to section observation, and film thickness is about 3 μ m, as shown in Figure 5.
The sample that embodiment 1 is made has been done energy spectrum analysis, and the content of chromium is 2.2wt%, as shown in Figure 6.
In embodiment 1, the magnetic control sputtering device of application is selected the MP700 model that Beijing praseodymium Ma Taike vacuum technology company limited produces.
Shown in Fig. 1, tungsten target material 7 is placed on the sputtering unit 1 of vacuum chamber 2,4 chromium targets 8 of 4 * 4 * 2mm specification are placed on to the maximum sputtering zone (dotted line) of tungsten target, 4 chromium targets 8 be take tungsten target material 7 centers and are put as symmetry, shown in Figure 1B.Cleaned tungsten substrate is placed in sample table 5.
The mass percent purity of tungsten target material is 99.999%, and the mass percent purity of tungsten substrate is 99.999%, and the mass percent purity of chromium target is 99.999%.
The pre-treatment of tungsten substrate: first tungsten substrate is placed in to deionized water and carries out ultrasonic cleaning 5 minutes, be placed in again alcohol (mass percent concentration is 70%) and carry out ultrasonic cleaning 5 minutes, be placed in again acetone (mass percent concentration is 99.5%) and carry out ultrasonic cleaning 5 minutes, be placed in again deionized water and carry out ultrasonic cleaning 5 minutes, be placed in again alcohol and carry out ultrasonic cleaning 5 minutes, take out, after seasoning, obtain clean rear tungsten substrate.The set of frequency of ultrasonic cleaning is 30KHz.
Close vacuum chamber, vacuum chamber 2 is vacuumized, make vacuum tightness in vacuum chamber 2 reach the back end vacuum values 5.5 * 10 of sputtering instrument
-4during Pa, to vacuum chamber 2, be filled with argon gas, argon flow amount is 19scc, and vacuum sputtering is pressed and is transferred to 0.9Pa; Adjusting sputter galvanic current is that 0.14A and dutycycle are 50.
Before deposition sputter, the first pre-sputtering of tungsten target 5 minutes, then regulates tungsten substrate in sample table 5 to the sputter area of radio frequency platform 1, and it is 8h that deposition sputtering time is set.
After sputter, closing device, takes out sample and carries out Performance Detection.
Sample that embodiment 2 is made adopts X-ray diffractometer to carry out material phase analysis to the chromium-doped W film of preparation, its peak value in [110], [200], [211], [220] overlap completely with tungsten base peak.
The sample that embodiment 2 is made is at electronic scanning electricity Microscopic observation, and film surface is smooth, and film thickness is about 3.5 μ m.
The sample that embodiment 2 is made is done energy spectrum analysis, and the content of chromium is 5.2wt%.
Shown in Fig. 1, tungsten target is placed on the sputtering unit 1 of vacuum chamber 2,6 chromium targets of 4 * 4 * 2mm specification are placed on to the maximum sputtering zone of tungsten target, 6 chromium targets be take tungsten target center and are put as symmetry.Cleaned tungsten substrate is placed in sample table 5.
The mass percent purity of tungsten target material is 99.999%, and the mass percent purity of tungsten substrate is 99.999%, and the mass percent purity of chromium target is 99.999%.
The pre-treatment of tungsten substrate: first tungsten substrate is placed in to deionized water and carries out ultrasonic cleaning 3 minutes, be placed in again alcohol (mass percent concentration is 70%) and carry out ultrasonic cleaning 3 minutes, be placed in again acetone (mass percent concentration is 99.5%) and carry out ultrasonic cleaning 2 minutes, be placed in again deionized water and carry out ultrasonic cleaning 5 minutes, be placed in again alcohol and carry out ultrasonic cleaning 5 minutes, take out, after seasoning, obtain clean rear tungsten substrate.The set of frequency of ultrasonic cleaning is 30KHz.
Close vacuum chamber, vacuum chamber 2 is vacuumized, make vacuum tightness in vacuum chamber 2 reach the back end vacuum values 4.6 * 10 of sputtering instrument
-4during Pa, to vacuum chamber 2, be filled with argon gas, argon flow amount is 21scc, and vacuum sputtering is pressed and is transferred to 0.7Pa; Adjusting sputter galvanic current is that 0.15A and dutycycle are 50.
Before deposition sputter, the first pre-sputtering of tungsten target 8 minutes, then regulates tungsten substrate in sample table 5 to the sputter area of radio frequency platform 1, and it is 7h that deposition sputtering time is set.
After sputter, closing device, takes out sample and carries out Performance Detection.
Sample that embodiment 3 is made adopts X-ray diffractometer to carry out material phase analysis to the chromium-doped W film of preparation, its peak value in [110], [200], [211], [220] overlap completely with tungsten base peak.
The sample that embodiment 3 is made is at electronic scanning electricity Microscopic observation, and film surface is smooth, and film thickness is about 2.8 μ m.
The sample that embodiment 3 is made is done energy spectrum analysis, and the content of chromium is 13.8wt%.
The present invention adopts magnetically controlled sputter method to prepare chromium-doped crystalline state W film, it is a kind of appropriate argon gas that is filled with in high vacuum chamber, between sputtering target negative electrode and substrate anode, apply galvanic current, tungsten target material and chromium target surface atom are sputtered out to the film forming method on tungsten substrate surface that is deposited on.It is low that magnetron sputtering method has temperature of reaction, and the physical bond power of coatings and substrate is strong, coatings is fine and close, the advantage such as even.Crystalline state Wu's thickness that the present invention makes reaches several microns, and the crystalline network that chromium element participates in tungsten grain completely forms, and at room temperature stable, need to, in the anneal of carrying out crystalline state, can not be directly used in the radiation research of hydrogen helium.
Claims (7)
1. a chromium-doped crystalline state W film, is characterized in that: the peak value of the crystalline state W film that this is chromium-doped is in [110], [200], [211], [220].
2. chromium-doped crystalline state W film according to claim 1, is characterized in that: the thickness of the crystalline state W film that this is chromium-doped is 2.5 microns～3.5 microns.
3. adopt magnetron sputtering technique to prepare a method for chromium-doped crystalline state W film, it is characterized in that there is the following step:
Step 1: the clean of tungsten substrate
The mass percent purity of tungsten substrate is 99.999%;
First tungsten substrate is placed in to deionized water and carries out ultrasonic cleaning 2～5 minutes, be placed in again alcohol (mass percent concentration is 70%) and carry out ultrasonic cleaning 2～5 minutes, be placed in again acetone (mass percent concentration is 99.5%) and carry out ultrasonic cleaning 2～5 minutes, be placed in again deionized water and carry out ultrasonic cleaning 2～5 minutes, be placed in again alcohol and carry out ultrasonic cleaning 2～5 minutes, take out, after seasoning, obtain clean rear tungsten substrate;
The set of frequency of ultrasonic cleaning is 30KHz;
Step 2: the placement of target and substrate
First tungsten target material is placed on the d.c. sputtering platform in magnetic control sputtering device vacuum chamber, then chromium target is placed on to the maximum sputtering zone of tungsten target;
Tungsten substrate after step 1 is cleaned is placed in the sample table in vacuum chamber;
Step 3: regulate sputtering pressure, sputter direct current
After substrate and footwear material are placed, close vacuum chamber, vacuum chamber is evacuated to back end vacuum 4 * 10
-4～5.5 * 10
-4pa;
Then, to vacuum chamber, be filled with argon gas, and to regulate argon flow amount and sputtering pressure, argon flow amount be 19～21scc, sputtering pressure is 0.7～0.9Pa; The volume percent purity of argon gas is 99.999%;
Then, regulate No Load Ratio 50 and sputter galvanic current 0.14～0.16A;
Step 4: magnetron sputtering made membrane
The splash-proofing sputtering process parameter setting according to step 3, opens run switch, after pre-sputtering 5～10min, regulates substrate to sputter area, and then, after magnetron sputtering deposition time 5～8h, closing device, takes out chromium-doped crystalline state W film.
4. employing according to claim 3 adopts magnetron sputtering technique to prepare the method for chromium-doped crystalline state W film, it is characterized in that: the specification of chromium target is 4 * 4 * 2mm, and the mode that chromium target is placed on tungsten target material is placed for symmetrical.
5. employing according to claim 4 adopts magnetron sputtering technique to prepare the method for chromium-doped crystalline state W film, it is characterized in that: the quantity of chromium target is 2,4 or 6.
6. employing according to claim 3 adopts magnetron sputtering technique to prepare the method for chromium-doped crystalline state W film, it is characterized in that: the peak value of the chromium-doped crystalline state W film making is in [110], [200], [211], [220].
7. employing according to claim 3 adopts magnetron sputtering technique to prepare the method for chromium-doped crystalline state W film, it is characterized in that: the chromium-doped crystalline state W film making thickness be 2.5 microns～3.5 microns.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070240981A1 (en) * | 2006-01-23 | 2007-10-18 | W. C. Heraeus Gmbh | Sputter Target With High-Melting Phase |
| CN102199756A (en) * | 2011-05-11 | 2011-09-28 | 北京航空航天大学 | Preparation method for amorphous tungsten film |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070240981A1 (en) * | 2006-01-23 | 2007-10-18 | W. C. Heraeus Gmbh | Sputter Target With High-Melting Phase |
| CN102199756A (en) * | 2011-05-11 | 2011-09-28 | 北京航空航天大学 | Preparation method for amorphous tungsten film |
Non-Patent Citations (1)
| Title |
|---|
| J. BHATTARAI, ET AL.: ""ELECTROCHEMICAL AND XPS STUDIES ON THE PASSIVATION BEHAVIOR OF SPUTTER-DEPOSITED W-Cr ALLOYS IN 12M HCl SOLUTION"", 《CORROSION SCIENCE》, vol. 40, no. 23, 31 December 1998 (1998-12-31), pages 155 - 175 * |
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Application publication date: 20140312 |