CN102199752B - Magneto-controlled sputter growing method for amorphous cadmium telluride thin films - Google Patents
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Abstract
The invention discloses a magneto-controlled sputter growing method for amorphous cadmium telluride thin films, which is characterized in that: in an ultrahigh vacuum magneto-controlled sputter growing chamber, the base vacuum degree is lower than 3.0*10<-4>Pa and the temperature is 25+/-10 DEG C; a high-purity cylindrical CdTe monocrystal target with a purity of 7N is used as a target material, high-purity Ar with a purity of 5N is used as a sputter working gas, and a glass slide is used as a substrate material; and the amorphous CdTe thin films are prepared respectively by a single-target common sputtering technique, a three-target intermittent sputtering technique or a two-target continuous and intermittent sputtering technique. The method has the advantages that: the process controllability is high; the production cost is low; and the industrial and large-scale production is easy. When the method is used, the amorphous CdTe thin films can be prepared at room temperature which is relatively low, the adhesivity of the prepared amorphous CdTe thin films is high, and the films are uniform in quality and compact.
Description
Technical field
The present invention relates to the room temperature magnetically controlled sputter method of non-crystalline state cadmium telluride (CdTe) film.
Background technology
Cadmium telluride (CdTe) is important II-VI group iii v compound semiconductor material.Regulate through suitable component proportion, CdTe can have N-shaped and two kinds of conduction types of p-type, the mobility of N-shaped CdTe and p-type CdTe current carrier is all better, its photoabsorption coefficient (to the light of wavelength less than ABSORPTION EDGE) is very big, thickness is the CdTe film of 1 μ m, can absorb the quantity of radiant energy greater than CdTe forbidden band energy 99%, therefore, the CdTe film has become the desirable absorption layer material of preparation high-level efficiency, low-cost solar cell, also is applicable to prepare the infrared optical element that the transmission wave band is 1～30 μ m.
Along with the development of s-generation Te-Cd-Hg (HgCdTe) infrared focus plane (FPA) thermal imaging system, the CdTe film is considered to a kind of desirable HgCdTe film surface passivating material.Because the requirement of HgCdTe device technology compatibility is diffusion and the loss that prevents Hg in the HgCdTe thin film layer, the growth of CdTe film must be carried out being lower than under 70 ℃ the condition, and this has brought larger difficulty for the CdTe thin film technology.At present, the CdTe film mainly adopts electro-deposition method, close-spaced sublimation method, closely the methods such as steam transport method, Vacuum sublimation prepare, its compactness of prepared film is bad, and under the room temperature deposition condition, the adhesivity of CdTe film and substrate surface has much room for improvement especially.Compare with polycrystalline, monocrystalline CdTe thin-film material, non-crystalline state CdTe film has the big area of being easy to deposition, structural uniformity is good, depositing temperature is low, the advantage that processing compatibility is good, at present, have no under room temperature (approximately 25 ℃ ± 10 ℃) processing condition and to adopt magnetically controlled sputter method to prepare non-crystalline state CdTe film.
Summary of the invention
The object of the present invention is to provide a kind of cost low, process controllability is strong, and is easy to the preparation method of the non-crystalline state CdTe thin-film material of commercial scale production, and is good to obtain adhesivity, the non-crystalline state CdTe thin-film material of membranous even compact satisfies the application demand of optoelectronic information device thin-film material.
Technical problem to be solved by this invention is: be in the sputter growth room under the condition of room temperature (25 ℃ ± 10 ℃), by three kinds of magnetron sputtering technique schemes, realize respectively the preparation of non-crystalline state CdTe rete.
The inventive method is achieved through the following technical solutions.
The primary condition of growth is: in the superhigh vacuum magnetron sputtering growth room with six station magnetron sputtering target position, the base vacuum degree is better than 3.0 * 10
-4Pa, temperature is 25 ℃ ± 10 ℃; Be that high-purity nahlock shape CdTe monocrystalline target of 7N is target with purity; Be that the high-purity Ar gas of 5N is the sputter working gas with purity; Be substrate material with slide glass, substrate material was used first the toluene ultrasonic cleaning 20 minutes, used the acetone ultrasonic cleaning 5～8 minutes again, removed the top layer organism, then used the dehydrated alcohol ultrasonic cleaning 5～8 minutes, removed the inorganics foreign ion, after taking out with 5N level N
2Air-blowing is done, and puts into the sputter growth room.
The conventional sputtering technology scheme of single target as realizing the growth of non-crystalline state CdTe thin-film material the steps include:
(1) being filled with Ar gas to vacuum tightness to the Grown by Magnetron Sputtering chamber is 1.0Pa～10Pa;
(2) open sputtering source, after build-up of luminance is stable, regulates sputtering power 8W～15W and (be equivalent to power density 0.28W/cm
2～0.53W/cm
2);
(3) will move to directly over the sputter target position as the slide glass directly over the non-sputter target position of being in of substrate, sputtering sedimentation CdTe rete, depositing time are 0.2～2 hour;
When (4) sputtering sedimentation finishes, rotate first the substrate rotating disk, remove substrate to non-sputter target position, close again shielding power supply, obtain non-crystalline state CdTe film.
Three target intermittent type sputtering technology schemes as realizing the growth of non-crystalline state CdTe thin-film material the steps include:
(1) being filled with Ar gas to vacuum tightness to the Grown by Magnetron Sputtering chamber is 1.0Pa～10Pa;
(2) select a CdTe film that the sputtering power condition of obvious crystallization has occured, namely (be equivalent to power density 0.530W/cm at 15W～30W
2～1.061W/cm
2) in the sputtering power scope, select a sputtering power;
(3) will move to as the slide glass directly over the non-sputter target position of being in of substrate directly over the sputter target position, sputtering sedimentation non-crystalline state CdTe rete, depositing time is 5～20 seconds, then rotate the substrate rotating disk, remove substrate, make substrate be in non-sputter target position 30～60 seconds (i.e. 30～60 seconds intermittences), finish the sputtering sedimentation of one-period, so repeat 30～120 sputtering sedimentation cycles;
When (4) sputtering sedimentation finishes, rotate first the substrate rotating disk, remove substrate to non-sputter target position, close again shielding power supply, obtain non-crystalline state CdTe film.
Two target sequencing batch sputtering technology schemes as realizing the growth of non-crystalline state CdTe thin-film material the steps include:
(1) being filled with Ar gas to vacuum tightness to the Grown by Magnetron Sputtering chamber is 1.0Pa～10Pa;
(2) selecting sputtering power is that 15W～30W (is equivalent to power density 0.530W/cm
2～1.061W/cm
2);
(3) selecting the revolution speed of substrate rotating disk is 1～5 week of per minute, in the time of directly over substrate enters the sputter target position, deposited amorphous attitude CdTe rete on the substrate, and directly over substrate produces the sputter target position time, without non-crystalline state CdTe thin film deposition, depositing time is 1～3 hour on the substrate;
When (4) sputtering sedimentation finishes, stop stepper-motor by computer program, close shielding power supply, obtain non-crystalline state CdTe film.
The invention has the beneficial effects as follows: under lower room temperature (25 ℃ ± 10 ℃) condition, realized non-crystalline state CdTe thin film technology; Adopt the non-crystalline state CdTe adhesion of film of the present invention's preparation good, membranous even compact; It is strong that the present invention has process controllability, and production cost is low, is easy to the advantage of commercial scale production.
Description of drawings
Fig. 1 is Grown by Magnetron Sputtering chamber schematic diagram;
Fig. 2 is non-crystalline state CdTe film " growth window " figure roughly;
Fig. 3 is the X-ray diffractogram of the non-crystalline state CdTe film of the conventional sputtering technology scheme growth of the single target of employing;
Fig. 4 is the X-ray diffractogram of the non-crystalline state CdTe film of employing three target intermittent type sputtering technology schemes growth;
Fig. 5 is the X-ray diffractogram of the non-crystalline state CdTe film of employing two target sequencing batch sputtering technology schemes growth.
Embodiment
Below in conjunction with accompanying drawing, by embodiment the present invention is described in further details, but protection scope of the present invention is not limited to the following examples.
Embodiment one:
The present embodiment is the situation that adopts the conventional sputtering technology scheme growth of single target non-crystalline state CdTe film.As shown in Figure 1, Grown by Magnetron Sputtering at FJL560III type ultrahigh vacuum(HHV) magnetic control and ionic fluid associating sputtering equipment is indoor, disk of placed horizontally, circumference in the disk certain radius is evenly distributed with six circular magnetron sputtering target position that size is identical, and defining clockwise the sputter target position is A, B, C, D, E, F.Directly over this disk, be provided with a substrate rotating disk coaxial with disk, be evenly distributed with the substrate bracket of six circles on the substrate rotating disk with on the isometrical circumference of magnetron sputtering target position, substrate bracket is corresponding one by one with size and the position of magnetron sputtering target position, and defining clockwise the substrate bracket Position Number is 1,2,3,4,5,6.Be designed with hollow shaft on the substrate rotating disk, the stepper-motor of computer program control can drive hollow shaft and rotate and then make the revolution of substrate rotating disk, and realization reaches the purpose of control substrate bracket target position of living in to the control of substrate bracket position.Six target position on the disk can be distinguished independent sputter CdTe target by six independently shielding power supply controls, at the substrate bracket position of six correspondences deposition CdTe film.Used sputtering target material is high-purity CdTe nahlock shape target of purity 7N.The sputter working gas high-purity Ar gas of purity 5N.Used substrate material is No. 7101 slide glasss of sailing boat board, thickness is 1mm approximately, substrate material was used first the toluene ultrasonic cleaning 20 minutes, used again the acetone ultrasonic cleaning 5～8 minutes, remove the top layer organism, then used the dehydrated alcohol ultrasonic cleaning 5～8 minutes, remove the inorganics foreign ion, do with 5N level N2 air-blowing after taking out, ultrasonic cleaning is with commercial ultrasonic cleaning machine.
The concrete technology step is: No. 7101 slide glass substrates that clean is crossed are put into the substrate bracket position No. 4, treat that the base vacuum degree of sputter growth room is better than 3 * 10
-4During Pa, in the sputter growth room, pass into 5N level Ar gas to 1.0Pa～10Pa, open A target magnetic control sputtering power supply, after build-up of luminance is stable, regulates sputtering power and from 8W to 15W, (be equivalent to power density 0.28W/cm
2～0.53W/cm
2), rotate the substrate rotating disk, regulate No. 7101 slide glass substrates of No. 4 substrate bracket positions to A target sputter position, sputtering sedimentation CdTe rete, depositing time are 0.5 hour, when sputtering sedimentation finishes, rotate first the substrate rotating disk, remove substrate to non-sputter target position, close again shielding power supply.
Take out the CdTe rete of sputtering sedimentation gained, the X-ray diffraction test draws the CdTe film for preparing on the substrate print and all shows amorphous structure (as shown in Figure 3).
By the CdTe rete of further test sputtering sedimentation gained, draw non-crystalline state CdTe film " growth window " scope roughly, as shown in Figure 2.With dashed lines connects article one line abbreviation " without the film line " of two open circles among Fig. 2, under experiment condition corresponding to these two soft dots, on the transparent slide glass without thin film deposition, characterize open circles line left side experiment condition without thin film deposition, and there is thin film deposition on the right side, be have film with without the line of delimitation of thin film deposition; The second line that with dashed lines connects solid pentagram among Fig. 2 is called for short " playing bright line ", these four solid pentagram points to part under, radio frequency source power only is added to when equaling sputtering power corresponding to solid pentagram, Ar gas just begins build-up of luminance and ionizes.It should be noted that fixedly sputtering pressure is 3Pa take (12W, 3Pa) point as reference, after the ionization of Ar gas build-up of luminance, suitably reducing sputtering power is 11W, 10W and three points of 9W, can form amorphous CdTe film, when sputtering power is reduced to 8W, without thin film deposition; With dashed lines connects the 3rd the line abbreviation " crystallization line " of five black triangles among Fig. 2, and under experiment condition corresponding to these five black triangle points, the CdTe film has shown that stronger crystallization diffraction peak is strong, and narrower diffraction peak width at half height.In the experimental point of Fig. 2, characterize that the left side experiment condition has the noncrystal membrane deposition or without thin film deposition, and the right side there is the crystallization thin film deposition, is roughly delineated out without film, amorphous, three membrane structure forms zones of crystallization by above-mentioned three experiment dotted lines.On the one hand the easier crystallization of magnetron sputtering C dTe film is described, on the other hand, this experiment " growth window " schematic diagram can be used for instructing magnetron sputtering non-crystalline state CdTe thin film technology.
Embodiment two:
The present embodiment is the situation that adopts three target intermittent type sputtering technology schemes growth non-crystalline state CdTe film.As shown in Figure 1, equipment used, material and processing are all identical with embodiment one, and different concrete technology steps are:
No. 7101 slide glass substrates that clean is crossed are put into 2,4, No. 6 three substrate bracket positions of sputter growth room, treat that the base vacuum degree of sputter growth room is better than 3 * 10
-4During Pa, in the sputter growth room, pass into 5N level Ar gas to 3.0Pa; Open the magnetron sputtering power supply of A, C, three sputter target position of E, after build-up of luminance is stable, regulates sputtering power and be 25W; Within each cycle, rotate the substrate rotating disk, regulate the substrate alignment of 2,4, No. 6 three substrate bracket positions to A, C, E target position, sputtering sedimentation CdTe film, depositing time are 10 seconds; Then rotate the substrate rotating disk, remove 2,4, No. 6 substrate brackets to non-sputter target position, make substrate be in non-sputter state 30 seconds, be i.e. at 30 seconds intermittences, be designated as one-period, so repeat 60 cycles; When sputtering sedimentation finishes, remove substrate to non-sputter target position, close shielding power supply.
Take out the CdTe rete of sputtering sedimentation gained, the X-ray diffraction test draws the CdTe film for preparing on three substrate prints and all shows amorphous structure (as shown in Figure 4).
Embodiment three:
The present embodiment is the situation that adopts two target sequencing batch sputtering technology schemes growth non-crystalline state CdTe film.As shown in Figure 1, equipment used, material and processing are all identical with embodiment one, and different concrete technology steps are:
No. 7101 slide glass substrates that clean is crossed are put into 2, No. 5 two substrate bracket positions of sputter growth room, treat that the base vacuum degree of sputter growth room is better than 3 * 10
-4During Pa, in the sputter growth room, pass into 5N level Ar gas to 3.0Pa; Open the magnetron sputtering power supply of A, two sputter target position of D, after build-up of luminance is stable, regulate sputtering power and be 25W, the revolution speed of regulating the substrate rotating disk is 3 weeks of per minute, setting depositing time is 2 hours, in the time of directly over substrate enters the sputter target position, and deposition CdTe film on the substrate, and directly over substrate produces the sputter target position time, on the substrate without the CdTe thin film deposition.When sputtering sedimentation finishes, stop stepper-motor by computer program, close shielding power supply.
Take out the CdTe rete of sputtering sedimentation gained, the X-ray diffraction test draws the CdTe film for preparing on two substrate prints and all shows amorphous structure (as shown in Figure 5).
Claims (4)
1. the Grown by Magnetron Sputtering method of non-crystalline state Cadimium telluride thin film, it is characterized in that: in the superhigh vacuum magnetron sputtering growth room with six station magnetron sputtering target position, the base vacuum degree is better than 3.0 * 10
-4Pa, temperature is 25 ℃ ± 10 ℃, is that high-purity nahlock shape CdTe monocrystalline target of 7N is target with purity, is that the high-purity Ar gas of 5N is the sputter working gas with purity, is substrate material with slide glass, puts into the sputter growth room, the steps include:
(1) being filled with Ar gas to vacuum tightness to the Grown by Magnetron Sputtering chamber is 1.0Pa～10Pa;
(2) open sputtering source, after build-up of luminance is stable, regulate sputtering power 8W～15W, be equivalent to power density 0.28W/cm
2～0.53W/cm
2
(3) will move to directly over the sputter target position as the slide glass directly over the non-sputter target position of being in of substrate, sputtering sedimentation CdTe rete, depositing time are 0.2～2 hour;
When (4) sputtering sedimentation finishes, rotate first the substrate rotating disk, remove substrate to non-sputter target position, close again shielding power supply, obtain non-crystalline state CdTe film.
2. the Grown by Magnetron Sputtering method of non-crystalline state Cadimium telluride thin film, it is characterized in that: in the superhigh vacuum magnetron sputtering growth room with six station magnetron sputtering target position, the base vacuum degree is better than 3.0 * 10
-4Pa, temperature is 25 ℃ ± 10 ℃, is that high-purity nahlock shape CdTe monocrystalline target of 7N is target with purity, is that the high-purity Ar gas of 5N is the sputter working gas with purity, is substrate material with slide glass, puts into the sputter growth room, the steps include:
(1) being filled with Ar gas to vacuum tightness to the Grown by Magnetron Sputtering chamber is 1.0Pa～10Pa;
(2) select a CdTe film that the sputtering power condition of obvious crystallization has occured, namely at 15W～30W, be equivalent to power density 0.530W/cm
2～1.061W/cm
2In the sputtering power scope, select a sputtering power;
(3) will move to as the slide glass directly over the non-sputter target position of being in of substrate directly over the sputter target position, sputtering sedimentation non-crystalline state CdTe rete, depositing time is 5～20 seconds, then rotate the substrate rotating disk, remove substrate, make substrate be in non-sputter target position 30～60 seconds, be i.e. 30～60 seconds intermittences, finish the sputtering sedimentation of one-period, so repeat 30～120 sputtering sedimentation cycles;
When (4) sputtering sedimentation finishes, rotate first the substrate rotating disk, remove substrate to non-sputter target position, close again shielding power supply, obtain non-crystalline state CdTe film.
3. the Grown by Magnetron Sputtering method of non-crystalline state Cadimium telluride thin film, it is characterized in that: in the superhigh vacuum magnetron sputtering growth room with six station magnetron sputtering target position, the base vacuum degree is better than 3.0 * 10
-4Pa, temperature is 25 ℃ ± 10 ℃, is that high-purity nahlock shape CdTe monocrystalline target of 7N is target with purity, is that the high-purity Ar gas of 5N is the sputter working gas with purity, is substrate material with slide glass, puts into the sputter growth room, the steps include:
(1) being filled with Ar gas to vacuum tightness to the Grown by Magnetron Sputtering chamber is 1.0Pa～10Pa;
(2) selecting sputtering power is 15W～30W, is equivalent to power density 0.530W/cm
2～1.061W/cm
2
(3) selecting the revolution speed of substrate rotating disk is 1～5 week of per minute, in the time of directly over substrate enters the sputter target position, deposited amorphous attitude CdTe rete on the substrate, and directly over substrate produces the sputter target position time, without non-crystalline state CdTe thin film deposition, depositing time is 1～3 hour on the substrate;
When (4) sputtering sedimentation finishes, stop stepper-motor by computer program, close shielding power supply, obtain non-crystalline state CdTe film.
4. according to claim 1, the Grown by Magnetron Sputtering method of 2 or 3 described non-crystalline state Cadimium telluride thin films, it is characterized in that using first the toluene ultrasonic cleaning 20 minutes as the slide glass of substrate material, used again the acetone ultrasonic cleaning 5～8 minutes, remove the top layer organism, then used the dehydrated alcohol ultrasonic cleaning 5～8 minutes, remove the inorganics foreign ion, use 5N level N after taking out
2Air-blowing is done, and puts into the sputter growth room again.
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| CN102925870A (en) * | 2012-10-26 | 2013-02-13 | 西安交通大学 | Preparation method of Zr-Cu-Ni-Al-Si metal amorphous film material |
| CN106222621B (en) * | 2016-08-23 | 2019-05-21 | 电子科技大学 | A kind of magnetic control sputtering device and magnetically controlled sputter method |
| CN107130210B (en) * | 2017-05-03 | 2019-09-20 | 中国建筑材料科学研究总院 | Surface is coated with the chalcogenide glass and preparation method thereof of infrared diamond-like protecting film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5393675A (en) * | 1993-05-10 | 1995-02-28 | The University Of Toledo | Process for RF sputtering of cadmium telluride photovoltaic cell |
| CN101168836A (en) * | 2006-10-25 | 2008-04-30 | 国家纳米技术与工程研究院 | Method for preparing bismuth telluride alloy thin film by employing cosputtering sedimentation method |
| CN101640233A (en) * | 2009-08-21 | 2010-02-03 | 四川阿波罗太阳能科技有限责任公司 | Device for producing CdS/CdTe solar cell by magnetron sputtering method |
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| AU2002349822B2 (en) * | 2001-10-05 | 2007-11-15 | Solar Systems & Equipments S.R.L. | A process for large-scale production of CdTe/CdS thin film solar cells |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5393675A (en) * | 1993-05-10 | 1995-02-28 | The University Of Toledo | Process for RF sputtering of cadmium telluride photovoltaic cell |
| CN101168836A (en) * | 2006-10-25 | 2008-04-30 | 国家纳米技术与工程研究院 | Method for preparing bismuth telluride alloy thin film by employing cosputtering sedimentation method |
| CN101640233A (en) * | 2009-08-21 | 2010-02-03 | 四川阿波罗太阳能科技有限责任公司 | Device for producing CdS/CdTe solar cell by magnetron sputtering method |
Non-Patent Citations (1)
| Title |
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| 周咏东等.CdTe的溅射生长及其对n-HgCdTe光导器件的表面钝化.《功能材料》.1998,第467-470页. * |
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