• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A method of growing a diamond crystal which comprises bombarding the diamond with a flux of carbon ions of sufficient energy to penetrate the diamond crystal and cause crystal growth which is at least predominantly internal, the temperature of the crystal being at least 400 DEG C. and less than the graphitization temperature, such that the diamond crystal structure is maintained during growth.
    公开号:SU1083915A3
    申请号:SU782624803
    申请日:1978-06-01
    公开日:1984-03-30
    发明作者:Стюарт Нельсон Ричард；Адриан Хадсон Джон；Джон Мейзи Дэвид
    申请人:Нэшнл Рисерч Дивелопмент Корпорейшн (Фирма)；
    IPC主号:
    专利说明:

    11 The invention relates to a method for producing semiconductor diamond. A known method of bombarding diamond at room temperature after annealing at twin temperatures. L Although bombardment at room temperature after annealing can be successful when silicon is used, it has been proved ineffective for diamond, since diamond structure transformed into amorphous carbon can be regenerated by simple heating. until the temperature is high, it is important that the bombardment be carried out while the crystal is at elevated temperatures. The closest to the present invention is a method for producing semiconductor diamond by treating it with a stream of carbon ions at room temperature followed by annealing of 2J. The radiation dose is low and diamond is such a good conductor of heat that the temperature rise during irradiation will be insignificant. Since the temperature does not reach, but is almost equal to the surrounding temperature, the diamond is transformed into an amorphous or phytic shape, and the electrical properties correspond to the fact that the diamond is gradually destroyed at a low dose of carbon incorporation. In addition, the presence of nitrogen in natural diamond adversely affects its semiconductor properties, to obtain (by simply bombarding natural diamonds with dopants. The purpose of the invention is to improve electrical properties. This goal is achieved because according to the method of producing semiconductor diamond by bombarding it with an ion flux Carbon process is carried out at 600-1075 C and carbon ion energy of 1-100 keV with simultaneous or subsequent bombardment by dopant ions. As a dopant, use Preferably, boron, phosphorus, mica, lithium or sodium ions are used. To obtain a pn-junction, a dopant of one type of conductivity is added to the flow of carbon ions, and the subsequent bombardment is led by dopant ions of the opposite type of conductivity .. 51 The process is carried out in a vacuum chamber at a pressure of 10 10 Torr. Dopants can be in a stream of carbon ions striking a crystalline target, usually in an amount not exceeding 0.1% of the flow, and in this case crystal growth and the introduction of The mixtures occur simultaneously and the impurity reports either conductivity of type p or conductivity of type p. Bombardment of a crystal with a stream of carbon ions and a stream of impurity ions can also occur alternately. In the latter case, the diamond layer is usually stripped, and then impurity ions are introduced by bombardment. These steps are repeated as necessary until the desired thickness is achieved, with the growth of the diamond layer with the impurity growing. In order to achieve a virtually uniform impurity concentration in the layer of grown diamond, its allowable thickness usually reaches no more than 1 OQ A and preferably no more than 50 A before introducing the impurity. Carbon ions, as well as impurity ions causing conductivities of type p or I on different ion sources, can be accelerated, as well as to combine these sources, if the bombardment is carried out simultaneously by different ions, before the ions hit the surface of the crystal, and as a rule, carried out independently of each other. Impurity ions whose masses are close to those of carbon, such as boron impurities, can be obtained and accelerated on the same emission machine. If it is necessary to obtain a p-transition, the crystal is bombarded with a stream of carbon ions containing an impurity that causes conductivity of either type p or type c, and then bombarded with ions causing another type of conductivity, and this bombardment is carried out with or without carbon ions. from the depth required for the transition and lying beneath the surface of the crystal. In this case, the bombardment conditions should be appropriately selected to eliminate the defect. caused by radiation and amorphous diamond. The dispersion rate, i.e. the number of atoms removed from the surface of the crystal upon the impact of an ion is less than unity, since otherwise the compression of the crystal subjected to bombardment would occur. The advantage of the proposed method is that the surface of the diamond being bombarded does not necessarily have to be perfect and can even be covered with a surface layer of a contaminating material. Therefore, as a rule, there is no need to resort to thorough cleaning methods, including, for example, the removal of grease and subsequent oxidation to obtain an ideal surface. In practice, carbon ions, as a rule, have a single charge and are the C-12 isotope, but they can also be another isotope. The energy of carbon ions and the additives used in the bombardment must be sufficient for the corresponding entry into the growing diamond crystal, and the entry distance must be at least 10 atomic sizes. Energy below 600 eV cannot provide the required insertion depth; this requires an energy of at least 1 keV, for example, 5-30 keV. Energy up to 100 keV gives satisfactory results. The temperature at which the transition from the crystalline state to the amorphous state occurs depends on the intensity of the flow of carbon ions; if the crystal temperature is too low, then there is a tendency to amorphization. If the temperature is at least 400 ° C, the diamond can be bombarded with an intensity that ensures the growth rate of the diamond to 0.1 mm / h. When temperatures are at least equal to 600 ° C, the intensity of the flow may be such as to give a growth rate of 3.2 mm / h. Although higher temperatures may allow the use of a higher flow intensity, the temperature of the onset of graphitization should not be exceeded. The graphitization temperature depends on the purity of the diamond sample and on the vacuum under which the sample is located; this temperature can be determined as a result of a simple experiment. Satisfactory results were obtained at 800 ° C or more, for example, the substrate can be heated to higher temperatures, but not Bbmie 1075 ° C. Using high temperatures allows the proposed method to be carried out without interruption to the annealing of the diamond target. Excessive heating, due to the very high flow rate, tends to damage the target, the current density, which determines the intensity of the flow, should be small, usually below 0.01 mA / cm. The upper boundary of the pressure in the chamber through which the ion flux passes (this stream usually has the shape of a beam) can be determined by the ability of the ion beam to cross the chamber and bombard the target, and the beat with the residual oxygen pressure in the chamber exerts an influence on the graphitization temperature. As a rule, this pressure does not exceed 10 Torr and preferably it is not higher. Despite the fact that in practice pressure cannot be above 10 Torr, it is usually inconvenient to reduce the pressure to below 10 Torr. A heavy ion accelerator can be used for bombardment. In the accelerator a boron ion beam can be formed, for example, from isolates of boron nitride at the source, which causes background contamination of the system. In a typical operation when the accelerator is turned on, the sample is irradiated with a beam of positive carbon ions with an energy of 30 keV, then the accelerating potential is changed to bring it to 32.5 keV, the magnet installation is kept constant, and the ions B are delivered as a beam to the irradiation site . The diamond can be grown with a thickness of 600 A, and then implanted until the desired crystal growth is achieved, usually 2 microns. Samples obtained with boron concentrations by growth layer contain on average 50, 160 and 345 ppm. Example 1. Introduction of boron impurity during the growth of an almae crystal The twin crystal is heated to a vacuum in the plane (ha) and alternately subjected to irradiation with C ions with an energy of 30 ke and boron ions with an energy of 32.5 keB. Irradiation with C ions and has the required intensity and duration in order to create diamond growth corresponding to 12 , 4 microns, in fact, with a uniform concentration of boron, is equal to approximately 330 h / ml. The increased part obtained at such crystallization shows all the characteristic features of natural diamond that occur during rotation during irradiation of the NIN with a pinch of C ions with energy. 30 keb. When testing four samples, it is determined that the layer obtained by growing is conductive and its resistance is in the order of 10 ohms / cm. Example 2. Growing a semiconductor layer with p-type conductivity. A triangular twin crystal with a side of 4 and a thickness of 1-2 mm is cleaned and placed on a graphite target, which is a heating zone. The bombarded crystal surface is polished and has orientation (III). A small area of the surface is covered by a mask, which is a graphite inhibitory coating; diamond is grown during the period of subsequent irradiation on a section without a graphite mask. The target area with a diamond crystal installed in it is located in the irradiation chamber of an accelerator of heavy ions so that the surface (W) with the mask applied to the diamond is located at a right angle to the ion beam coming from the source. In the chamber with the target, the residual pressure is brought to a level of 10 Torr and the sample is heated to 800 C. Then the sample is alternately bombarded with C and B ions with an energy of 30 keb while maintaining the temperature during ion bombardment at 800 + 20 C. The time period during which the B ions are bombarded, are chosen so as to obtain on average an Ion B concentration equal to 300 ppm. The time for implantation of C ions is taken so that each step of approximately 500 amps is carried out between each implantation B. The sample is cooled to ambient temperature, removed from the irradiation zone and cleaned. The measured increase in thickness due to growth is 2 mm. The sample is heat treated under vacuum for 15 min at 1500 ° C and cooled to ambient temperature. Electrical tests (on points and a thermal sample) on the surface of a crystal subjected to bombardment allow us to establish that the resistance of a flat sample is approximately 1 X 10 per square, and also to establish the presence of p-type carriers. Conductivity was not detected when testing at four points on a polished surface (W), not subjected to the bombardment of a twinned diamond crystal. ; The presence of boron in the grown crystal was confirmed by mass spectroscopy of the secondary ion. The crystal under study was placed in a Sámez device and on a small surface area with a structure (Ø) bombarded with oxygen ions having an energy of 2 keV, molecules were pulled from the sample placed in the target zone. Boron is found in knocked out molecules all over the grown layer.
    权利要求:
    Claims (4)
    [1]
    1. METHOD FOR PRODUCING SEMICONDUCTOR DIAMOND by bombarding it with a stream of carbon ions, characterized in that, in order to improve electrical properties, the process is conducted at 600-1075 ° C and carbon ion energy of 1-100 keV with simultaneous or subsequent bombardment by dopant ions.
    [2]
    2. The method of pop. ^ characterized in that boron, phosphorus, arsenic, lithium or sodium ions are used as the dopant.
    [3]
    3. The method according to PP. 1 and 2, characterized in that, in order to obtain a p-h junction, a dopant of one type of conductivity is added to the flow of carbon ions, and the subsequent bombardment is carried out by dopant ions of the opposite type of conductivity.
    [4]
    4. The method according to PP. 1-3, which is consistent with the fact that the process is conducted in a vacuum chamber at a pressure of 10 '^ 10 * 9 TO pp,
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    同族专利:
    公开号 | 公开日
    GB1599668A|1981-10-07|
    CA1098219A|1981-03-24|
    US4277293A|1981-07-07|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    CA727830A|1966-02-08|General Electric Company|Rectifiers made from p-type semiconductors|
    NL281867A|1961-08-09|
    US3142595A|1961-08-31|1964-07-28|Gen Electric|Bulk junctions employing p-type diamond crystals and method of preparation thereof|
    US3383567A|1965-09-15|1968-05-14|Ion Physics Corp|Solid state translating device comprising irradiation implanted conductivity ions|
    US3630679A|1968-06-26|1971-12-28|Univ Case Western Reserve|Diamond growth process|
    US3961103A|1972-07-12|1976-06-01|Space Sciences, Inc.|Film deposition|
    US4191735A|1973-06-07|1980-03-04|National Research Development Corporation|Growth of synthetic diamonds|US4495044A|1983-05-17|1985-01-22|The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration|Diamondlike flakes|
    US4571447A|1983-06-24|1986-02-18|Prins Johan F|Photovoltaic cell of semi-conducting diamond|
    JPH0346436B2|1986-10-23|1991-07-16|Kagaku Gijutsucho Mukizaishitsu Kenkyushocho|
    US4929489A|1987-07-20|1990-05-29|Dreschhoff Gisela A M|Method of making and using selective conductive regions in diamond layers|
    US5051785A|1989-06-22|1991-09-24|Advanced Technology Materials, Inc.|N-type semiconducting diamond, and method of making the same|
    CA2021020A1|1989-07-13|1991-01-14|Johan Frans Prins|Diamond diode structure|
    US5141460A|1991-08-20|1992-08-25|Jaskie James E|Method of making a field emission electron source employing a diamond coating|
    US5129850A|1991-08-20|1992-07-14|Motorola, Inc.|Method of making a molded field emission electron emitter employing a diamond coating|
    US5334283A|1992-08-31|1994-08-02|The University Of North Carolina At Chapel Hill|Process for selectively etching diamond|
    US5410166A|1993-04-28|1995-04-25|The United States Of America As Represented By The Secretary Of The Air Force|P-N junction negative electron affinity cathode|
    US5609926A|1994-03-21|1997-03-11|Prins; Johan F.|Diamond doping|
    JPH09106958A|1995-06-23|1997-04-22|De Beers Ind Diamond Div Ltd|Doping of crystal substrate|
    AU1155502A|2000-10-09|2002-04-22|Univ Chicago|N-type doping of nanocrystalline diamond films with nitrogen and electrodes madetherefrom|
    US6793849B1|2000-10-09|2004-09-21|The University Of Chicago|N-type droping of nanocrystalline diamond films with nitrogen and electrodes made therefrom|
    US6753469B1|2002-08-05|2004-06-22|The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration|Very high efficiency, miniaturized, long-lived alpha particle power source using diamond devices for extreme space environments|
    US20070062300A1|2003-09-25|2007-03-22|Dorfman Benjamin F|Method and apparatus for straining-stress sensors and smart skin for air craft and space vehicles|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    GB23468/77A|GB1599668A|1977-06-02|1977-06-02|Semiconductors|
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