CN1289867A - Hot liquid method for growing monocrystal of gallium nitride - Google Patents
Hot liquid method for growing monocrystal of gallium nitride Download PDFInfo
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- CN1289867A CN1289867A CN 99119719 CN99119719A CN1289867A CN 1289867 A CN1289867 A CN 1289867A CN 99119719 CN99119719 CN 99119719 CN 99119719 A CN99119719 A CN 99119719A CN 1289867 A CN1289867 A CN 1289867A
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Abstract
A hot liquid method for growing monocrystal of gallium mitride features that the monocrystal of gallium nitride is grown in a temp field at 400-600 deg.C and 1000-1800 Pa in the high-pressure reactor with liner of inertical material. Said temp field is provided by a temp control system. Its advantages include simple equipment, low cost, high output rate. The diameter of said monocrystal is greater than 20 microns and its length is mm class.
Description
The present invention relates to a kind of growing method, particularly relate to a kind of growth method of gallium nitride single crystal.
GaN is excellent wide bandgap semiconductor materials, and its room temperature band gap is wide to be 3.4eV, is the ideal material of manufacturing indigo plant, green photodiode and laser diode.This class light source has a wide range of applications and huge economic benefit at aspects such as optical information storage, high-rate laser printing, light demonstration, acquisition of signal and medical science.
Mostly be at present to adopt MOCVD (metal organic chemical vapour deposition) to produce the GaN semiconductor film, make laser diode, for example, use hydrogen carrier (hydrogen carrier gas) trimethyl-gallium, ammonia (NH
3) and the gas of dicyclopentadienyl magnesium (bis-cyclopentadienyl magnesium) supply with the white stone substrate.Substrate is heated to 1000 ℃, makes the above-mentioned raw materials gas reaction, forms the GaN film of mixing magnesium on substrate surface.Shine this film with low-energy electron beam after growing into film, to obtain p N-type semiconductorN (document 1.H.Amano, et al.Jpn.J.Appl.Phys.Vol.28 (1989) L2112).As everyone knows, the equipment price of MOCVD is very high, and output is little, is difficult to reduce production costs, and realizes real large-scale commercial production.Simultaneously, the lowest order dislocation density of the epitaxially deposited layer of this GaN is unexpectedly up to 10
8/ cm
2In all known substrate materials, the GaN single crystalline substrate is to produce the best substrate of blue light laser diode.The isoepitaxial growth of carrying out on the single crystal of gan is the preferred approach that reduces this dislocation desity.In addition, directly making diode on gallium nitride single crystal, is the optimal path of making blue light laser diode.So the growing large-size gallium nitride single crystal is extremely important.But the piece monocrystalline of gan but can not melt the body from stoichiometry with existing method such as caochralski or Bridgman grows, and this mainly is because the temperature of fusion of gan is high, and has very high balance decomposition pressure when fusion.General melting the requirement that the attitude growth apparatus all can not satisfy such harshness, the crystal of growing semiconductor quality almost be impossible under such temperature and pressure.Thereby the gallium nitride single crystal body must be grown with the method that can reduce growth temperature.
S.Porowski of Poland and I.Grzegoryz (document 2.J.Cryst.GrowthVol.178 (1997) p.174) disclose at high temperature a kind of, from being full of high pressure N
2The Ga solution system in the method for growth sheet GaN monocrystalline, its temperature and pressure is respectively up to 1400-1600 ℃ with the 10-20 kilobar.So unusual Ke Ke processing condition, common laboratory all are difficult to realize, have said nothing of industrialized mass production.
The Chen Xiaolong of China etc. has proposed a kind of hot liquid method for growing of growing gallium nitride powder, has grown gan nano-powder (document 3. old little dragons etc., Chinese invention patent, application number 98125641.4) under 300-400 ℃ lesser temps.Make the GaN film on the substrate and make the Nano semiconductor device because this kind powder is suitable for being sprayed on, therefore the substrate material that can not be directly use as isoepitaxial growth and make laser diode is necessary to seek a kind of method of the monocrystalline of growing GaN at low temperatures.
The people such as R.Dwilinski of Poland (document 4.Acta Phys.Pol., A Vol.90 (1996) 763; Vol.88 (1995) 833) Ga and liquid NH
3Pack in the autoclave, at LiNH
2Or K does under the condition of mineralizer, grows GaN when being lower than 500 ℃ and 5Kbar.Though have the monocrystalline that reaches 25 μ m to occur, product mainly is GaN powder and class stupalith, the monocrystalline productive rate is very low.
The A.P.Purdy of the U.S. (document 5.Chem.Mater.Vol.11 (1999) 1648) in silica tube, uses NH
3With metal Ga, at NH
4Under the mineralizer effect of I, under 10000psi and about 500 ℃ condition, on quartzy tube wall, grow Cubic GaN and the six side GaN monocrystalline of 4 μ m.Purdy also uses NH
4Br and NH
4Cl makes mineralizer, with GaI and NH
3Similarly generating the GaN deposited film under the condition.But the monocrystalline size that grows less (about 4 μ m) only can be used for the usefulness of scientific research, and does not have too big using value.
The objective of the invention is to overcome the shortcoming of prior art, by on the internal chamber wall of autoclave, adding attached lining, and utilize temperature controlling system that a temperature is provided, thereby in hydrothermal solution, grow gallium nitride single crystal.Temperature and pressure of the present invention is all not too high, equipment is simple, with low cost and efficient, be convenient to industrialized mass production GaN monocrystal material.The diameter of the gallium nitride single crystal that grows is greater than 20 μ m, and length is the millimeter magnitude, and productive rate is higher.
The object of the present invention is achieved like this:
1. high purity metal gallium 6, halogenation ammonia salt 10, high-purity liquefied ammonia 5 and the internal chamber wall that will intend participating in reaction all packed into the autoclave body 2 of lining 8 and sealing plug 1 thereof, seal cap 3 in the vacuum glove box, and bleeds and make the vacuum tightness of this glove box reach 10
-2Torr, to remove aqueous vapor and airborne oxygen, lining material is not for reacting and can suppress the inert material of the excessive nucleation of gan with gallium, as platinum, gold, iridium, BN, AlN etc., in order to make liquefied ammonia 5 unlikely rapid vaporizations, used here autoclave body 2 is put into vacuum glove box in advance again after cooled with liquid nitrogen is handled.
2. in vacuum glove box, by 8: 2～9: 1 molar ratio weighing high purity metal galliums 6 and halogenation ammonia salt 10 (as NH
4Cl, NH
4Br, NH
4F or NH
4I), in the autoclave body 2 of packing into then, wherein halogenide ammonia salt 10 plays a part mineralizer.
3. pour high-purity liquefied ammonia 5 into by 65～90% degree of filling.
4. immediately sealing plug 1 and seal cap 3 are contained on the autoclave body 2, tighten, and tentatively seal, scatter and disappear for the vaporization of avoiding high-purity liquefied ammonia 5 as far as possible, all operations all should carry out rapidly.
5. on the seal operation platform, autoclave is done further to seal.
6. the autoclave of sealing is taken out, put into a two-part resistance heading furnace 4, by thermopair 7 control heat temperature raising to 400～600 ℃, and utilize temperature controlling system to make in the autoclave thermograde up and down be 20-50 ℃, required motivating force when this temperature difference has produced the monocrystalline crystallization.
7. constant temperature is 3～6 days, can obtain water white hexagonal columnar product 9 on the middle part or the top of autoclave, and its diameter is greater than 20 μ m, and length is the millimeter magnitude, through the identification of phases of powder X-ray ray thing, confirms as the GaN monocrystalline.
The temperature and pressure of growing gallium nitride single crystal of the present invention all not too high (temperature is 400-600 ℃, and pressure is the 1000-1800 crust), its condition is fit to laboratory and industrial production, and equipment is simple, and gan productive rate height is fit to industrialized mass production.The monocrystalline size that grows reaches a millimeter magnitude, has great practical value.
The present invention will be described in detail below in conjunction with drawings and Examples:
Fig. 1 is the hydrothermal solution reactive system synoptic diagram of growing GaN monocrystalline,
Fig. 2 is the X-ray powder diffraction spectrum of the GaN monocrystalline that grows,
Fig. 3 is the photo in kind of the GaN monocrystalline that grows,
Wherein: 1 sealing plug, 2 autoclave bodies, 3 seal caps, 4 resistance heading furnaces
5 high-purity liquefied ammonia 6 high purity metal galliums 7 thermopairs 8 linings
9GaN monocrystalline 10 halogenation ammonia salt
Embodiment 1
With the high purity metal gallium of waiting to participate in reacting 6, analytically pure NH
4High-purity liquefied ammonia 5 of Cl10 and 50 milliliters and internal diameter are that the integral unit of autoclave of the chilled band BN lining of Φ 15mm is put into vacuum glove box, vacuumize the vacuum tightness that makes in the glove box and reach 10
-2Torr.In vacuum glove box, take by weighing the high purity metal gallium 6 of 3.15 grams and the NH of 0.27 gram by 9: 1 mol ratios
4Cl10 packs in the autoclave body 2, and pours 540 milliliters in liquefied ammonia into by 65% degree of filling, and in order to make liquefied ammonia 5 unlikely rapid vaporizations, used here autoclave is to handle through cooled with liquid nitrogen in advance.Be contained in the sealing plug 1 of autoclave and seal cap 3 on the autoclave body 2 fast and tighten, in addition tentatively sealing.For the lost all operations of the vaporization of avoiding liquefied ammonia 5 all should carry out rapidly as far as possible.The autoclave that installs is taken out, on the seal operation platform autoclave is done further sealing, afterwards the autoclave of sealing is put into two-part resistance heading furnace 4 and be warming up to 500 ℃, upper and lower temperature difference is 100 ℃.Constant temperature promptly obtained water white hexagonal columnar crystal in 5 days in autoclave, be the GaN monocrystalline through the identification of phases of X ray thing.
With the high purity metal gallium of waiting to participate in reacting 6, analytical pure NH
4F10, high-purity liquefied ammonia 5 and internal diameter are that the tubulose autoclave integral unit of the band platinum lining of Φ 15mm is put into a vacuum glove box, and the vacuum tightness of finding time to make this glove box is for to 10
-2Torr.In vacuum glove box, take by weighing the high purity metal gallium 6 of 4.17 grams and the NH of 0.39 gram by 17: 3 mol ratios
4F10 packs in the autoclave body 2, pours liquefied ammonia 5 into by 70% degree of filling, and in order to make liquefied ammonia 5 unlikely rapid vaporizations, employed here autoclave body 2 is to handle through cooled with liquid nitrogen in advance, for the vaporization of avoiding liquefied ammonia 5 all operations that scatters and disappears all should carry out rapidly as far as possible; Be contained in the sealing plug 1 of autoclave and seal cap 3 on the autoclave body 2 and tighten, in addition tentatively sealing.The autoclave that installs is taken out, on the seal operation platform autoclave is done further sealing, the autoclave that is about to seal is afterwards put into two-part resistance heading furnace 4 and is warming up to 400 ℃, and upper and lower temperature difference is 20 ℃.Constant temperature promptly obtained water white hexagonal columnar crystal in 4 days on the top of autoclave, be the GaN crystal through material phase analysis.
Embodiment 3
With the high purity metal gallium of waiting to participate in reacting 6, analytical pure NH
4Br10, high-purity liquefied ammonia 5 and internal diameter are that the tubulose autoclave integral unit of the band gold lining of Φ 15mm is put into a vacuum glove box, and the vacuum tightness of finding time to make this glove box is for to 10
-2Torr.Mol ratio by 4: 1 in vacuum glove box takes by weighing the high purity metal gallium 6 of 4.17 grams and the NH of 1.46 grams
4Br10 packs in the autoclave body 2, pours liquefied ammonia 5 into by 90% degree of filling, and in order to make liquefied ammonia 5 unlikely rapid vaporizations, employed here autoclave is to handle through cooled with liquid nitrogen in advance, scatters and disappears for the vaporization of avoiding liquefied ammonia 5 as far as possible, and all operations all should carry out rapidly; Be contained in the sealing plug 1 of autoclave and seal cap 3 on the autoclave body 2 and tighten, in addition tentatively sealing.The autoclave that installs is taken out, on the seal operation platform autoclave is done further sealing, the autoclave that is about to seal is afterwards put into two-part resistance heading furnace 4 and is warming up to 600 ℃, and upper and lower temperature difference is 150 ℃.Constant temperature promptly obtained water white hexagonal columnar crystal in 4 days in autoclave, be the GaN crystal through material phase analysis.
Embodiment 4
With the high purity metal gallium of waiting to participate in reacting 6, analytically pure NH
4I10, high-purity liquefied ammonia 5 and internal diameter are that the tubulose autoclave integral unit of the band AlN lining of Φ 15mm is put into a vacuum glove box, and the vacuum tightness of finding time to make this glove box is for to 10
-2Torr.Mol ratio by 4: 1 in vacuum glove box takes by weighing the high purity metal gallium 6 of 4.10 grams and the NH of 1.64 grams
4I10 packs in the autoclave body 2, pours liquefied ammonia 5 into by 70% degree of filling, and in order to make liquefied ammonia 5 unlikely rapid vaporizations, employed here autoclave is to handle through cooled with liquid nitrogen in advance, scatters and disappears for the vaporization of avoiding liquefied ammonia 5 as far as possible, and all operations all should carry out rapidly; Be contained in the sealing plug 1 of autoclave and seal cap 3 on the autoclave body 2 and tighten, in addition tentatively sealing.The autoclave that installs is taken out, on the seal operation platform autoclave is done further sealing, the autoclave that is about to seal is afterwards put into two-part resistance heading furnace 4 and is warming up to 450 ℃, and upper and lower temperature difference is 75 ℃.Constant temperature promptly obtained water white hexagonal columnar crystal in 6 days in autoclave, be the GaN crystal through material phase analysis.
Be noted that the above embodiments just illustrate the present invention with four concrete examples, it should not be a limitation of the present invention.Simultaneously, be familiar with all knowing of this technology, can carry out in the text the not various improvement of description to the present invention, and these improve the spirit and scope that can not depart from this patent.
Claims (3)
1, a kind of hot liquid method for growing of gallium nitride single crystal is characterized in that: may further comprise the steps:
(1) high purity metal gallium (6), halogenation ammonia salt (10), high-purity liquefied ammonia (5) and the internal chamber wall that will intend participating in reaction has the autoclave body (2) of lining (8) and sealing plug (1) thereof, seal cap (3) and all packs in the vacuum glove box, and bleeds and make the vacuum tightness of this glove box reach 10
-2Torr, used lining are inert material, and used autoclave body is handled through cooled with liquid nitrogen in advance;
(2) in vacuum glove box, by 8: 2～9: 1 molar ratio weighing high purity metal gallium (6) and halogenation ammonia salt (10);
(3) pour high-purity liquefied ammonia (5) into by 65～90% degree of filling;
(4) immediately sealing plug (1) and seal cap (3) are contained on the autoclave body (2), tighten, and tentatively seal, all operations all is to carry out fast;
(5) on the seal operation platform, autoclave is done further to seal;
(6) autoclave sealed is taken out, put into a two-part resistance heading furnace (4),, and utilize temperature controlling system to make in the autoclave thermograde up and down be 20-150 ℃ by thermopair (7) control heat temperature raising to 400～600 ℃;
(7) constant temperature is 3～6 days, can obtain water white hexagonal columnar product (9) on the middle part or the top of autoclave.
2, by the hot liquid method for growing of the described gallium nitride single crystal of claim 1, it is characterized in that: the lining of autoclave internal chamber wall (8) can be platinum, gold, iridium, BN or AlN.
3, by the hydrothermal solution reaction method of the described gallium nitride single crystal of claim 1, it is characterized in that: used halogenation ammonia salt (10) can be NH
4Cl, NH
4Br, NH
4F or NH
4I.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99119719 CN1113988C (en) | 1999-09-29 | 1999-09-29 | Hot liquid method for growing monocrystal of gallium nitride |
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|---|---|---|---|
| CN 99119719 CN1113988C (en) | 1999-09-29 | 1999-09-29 | Hot liquid method for growing monocrystal of gallium nitride |
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1999
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