CN108950504A - A kind of alloy target material and preparation method thereof forming Ohmic contact on N-type compound semiconductor materials surface - Google Patents

A kind of alloy target material and preparation method thereof forming Ohmic contact on N-type compound semiconductor materials surface Download PDF

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CN108950504A
CN108950504A CN201810874089.2A CN201810874089A CN108950504A CN 108950504 A CN108950504 A CN 108950504A CN 201810874089 A CN201810874089 A CN 201810874089A CN 108950504 A CN108950504 A CN 108950504A
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indium
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ohmic contact
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CN108950504B (en
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Jiangsu Huanhao Metal Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C28/00Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering

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Abstract

A kind of alloy target material and preparation method thereof forming Ohmic contact on N-type compound semiconductor materials surface.More particularly to a kind of indium silver-gold alloy target material and preparation method thereof for forming Ohmic contact on N-type compound semiconductor materials surface.Provide that a kind of adhesion is good, plasticity is good, the simple indium silver-gold alloy target material of preparation method and preparation method thereof.The present invention can directly form good Ohmic contact in gallium arsenide surface compared to gold-germanium alloy, using indium silver-gold alloy target material.Meanwhile using the elongation after fracture of indium billon made from preparation method of the present invention up to 23.5-30%, plasticity is good, can be processed into required shape according to the demand of different occasions.

Description

A kind of alloy target material forming Ohmic contact on N-type compound semiconductor materials surface And preparation method thereof
Technical field
The present invention relates to the preparation methods of alloy target material, and in particular to one kind is in N-type compound semiconductor materials surface shape At the indium silver-gold alloy target material and preparation method thereof of Ohmic contact.
Background technique
Excellent metal semiconductor Ohmic contact, for manufacturing opto-electronic device, microwave oscillator with compound semiconductor And the parameter and stability of microwave circuit are extremely important, and for GaAs (GaAs) material, generally common gold germanium (AuGe) alloy Form good Ohmic contact, preparation process be the co-melting body of AuGe is vaporized on GaAs, and using short annealing technology into Row Alloying Treatment.In alloying process, Ge(germanium) quickly diffusion couple GaAs progress heavy N-type doping, in metal and semiconductor Between formed electron tunnel break-through without generate potential barrier.Currently, being existed under optimal technique using electrode prepared by gold-germanium alloy Specific contact resistivity can reach 5.8 × 10 on N-type GaAs material-7Ω·cm2.Although obtaining good effect, gold-germanium alloy There are still some problems in terms of preparing Ohmic contact: (1) firstly, when being processed gold-germanium alloy to prepare sputtering target material It was found that the alloy brittleness is larger, processing performance is poor.The method for usually preparing gold-germanium alloy sputtering target material is that casting is advised with target Ingot casting similar in lattice, hypoeutectic or eutectic structure when thus obtained gold-germanium alloy target microstructure is as cast condition, is unfavorable for Obtain final high performance thin film.(2) in addition, gold-germanium alloy has to pass through short annealing process, in semiconductor material surface and arsenic Change gallium material to react to form alloy polarizing electrode, high-performance Ohmic electrode can be formed.Therefore, one kind is selected to be easily worked, and The simple metal electrode technique of preparation process is particularly important.
Summary of the invention
The present invention is in view of the above problems, provide that a kind of adhesion is good, plasticity is good, the simple indium billon target of preparation method Material and preparation method thereof.
The technical scheme is that
A kind of alloy target material forming Ohmic contact on N-type compound semiconductor materials surface, including following component: 2-8 wt% Gold and 92-98 wt% indium.
A kind of preparation method for the alloy target material forming Ohmic contact on N-type compound semiconductor materials surface, including such as Lower step:
1), indium metal is melted using vacuum induction melting furnace, then gold nano powder is mixed into the indium metal of molten condition And it stirs evenly;
2), melt under agitation, keeps the temperature degasification 15-20 minutes;
3) indium gold mixed liquor, is poured into mold at a temperature of 180-220 DEG C, is cooled to room temperature, indium billon ingot casting is formed;
4) ingot casting, is subjected to hot pressing rolling processing, removes internal porosity and crystal boundary;
5) it is small that the alloy cast ingot after, being processed using heating furnace to hot pressing rolling homogenizes heat treatment 1-5 at a temperature of 80-120 DEG C When;
6), ingot casting is cut using linear cutting equipment;
7), the ingot casting after being thinned is polished, essence throws and forms target.
Indium metal melting condition in the step 1) are as follows:, will in the vacuum induction melting furnace that vacuum degree is 8-12 Pa Indium raw material are heated to 200-220 DEG C, after indium metal all melts, keep the temperature 30-40 minutes.
Hot pressing rolling condition in the step 4) is 45-55 DEG C.
It is 3-8% that the ingot casting, which carries out hot pressing rolling pass deformation rate,.
The beneficial effects of the present invention are: the work function of indium is very close with GaAs conduction band, if by indium preparation and arsenic Gallium surface will form good electron transfer layer, while since energy band matches in order to improve indium in the nucleation energy of gallium arsenide surface Power adds the golden material of proper proportion in phosphide material, increase in coating process metal material gallium arsenide film surface at Nuclear capability.At room temperature, good Europe is formed in N-type gallium arsenide surface by indium gold alloy electrodes prepared by magnetically controlled sputter method Nurse contact, ohmic contact resistance can be down to 5.6 × 10-7Ω·cm2, have the effect of that same gold germanium target is similar, simultaneously because making Complicated short annealing process is needed not move through with indium silver-gold alloy target material, therefore compared to gold-germanium alloy, uses indium billon target Material can directly form good Ohmic contact in gallium arsenide surface.Meanwhile utilizing indium billon made from preparation method of the present invention Elongation after fracture up to 23.5-30%, plasticity is good, can be processed into required shape according to the demand of different occasions.
Detailed description of the invention
Fig. 1 is that GaAs material surface is prepared with indium billon shape appearance figure,
Fig. 2 is the edge pattern SEM figure for the electrode that spacing is 20 μm.
Specific embodiment
The present invention is illustrated below with reference to embodiment.
Embodiment 1
The target is mixed by 2 wt% gold and 98 wt% indiums, and the preparation method includes the following steps:
1), using vacuum induction melting furnace that indium metal melting is (former by indium in the vacuum induction melting furnace that vacuum degree is 8 Pa Material is heated to 200 DEG C, after indium metal all melts, keeps the temperature 30 minutes), then gold nano powder (10-100nm) is mixed into In the indium metal of molten condition and stir evenly;
2), melt under agitation, keeps the temperature degasification 15 minutes;
3) indium gold mixed liquor, is poured into mold at a temperature of 180 DEG C, is cooled to room temperature (15-30 DEG C), eutectic composition or Asia are formed The indium billon ingot casting of eutectic composition;
4), by ingot casting progress hot pressing rolling processing, (45 DEG C, hot rolling pass deformation rate is 3%), to remove internal porosity and crystal boundary;
5) heat treatment 5 hours, is homogenized at a temperature of 80 DEG C to the alloy cast ingot after hot pressing rolling processing using heating furnace;
6), ingot casting is cut using linear cutting equipment, realizes that thickness is thinned;
7), the ingot casting after being thinned is polished, essence throwing forms target, and (by taking four inches of targets as an example: diameter is about 100mm, thick Spend 10mm, round or square), obtain sample 1.
Embodiment 2
The target is mixed by 8 wt% gold and 92 wt% indiums, and the preparation method includes the following steps:
1), using vacuum induction melting furnace that indium metal melting is (former by indium in the vacuum induction melting furnace that vacuum degree is 12Pa Material is heated to 220 DEG C, after indium metal all melts, keeps the temperature 40 minutes), gold nano powder is then mixed into molten condition In indium metal and stir evenly;
2), melt under agitation, keeps the temperature degasification 20 minutes;
3) indium gold mixed liquor, is poured into mold at a temperature of 220 DEG C, is cooled to room temperature, eutectic composition or hypoeutectic ingredient are formed Indium billon ingot casting;
4), by ingot casting progress hot pressing rolling processing, (55 DEG C, hot rolling pass deformation rate is 8%), to remove internal porosity and crystal boundary;
5) heat treatment 1 hour, is homogenized at a temperature of 120 DEG C to the alloy cast ingot after hot pressing rolling processing using heating furnace;
6), ingot casting is cut using linear cutting equipment, realizes that thickness is thinned;
7), the ingot casting after being thinned is polished, essence throws and forms target, and anneal 10s under the conditions of 50 DEG C, obtains sample 2.
Embodiment 3
The target is mixed by 5 wt% gold and 95 wt% indiums, and the preparation method includes the following steps:
1), indium metal is melted (in the vacuum induction melting furnace that vacuum degree is 10 Pa, by indium using vacuum induction melting furnace Raw material are heated to 210 DEG C, after indium metal all melts, keep the temperature 32 minutes), gold nano powder is then mixed into molten condition Indium metal in and stir evenly;
2), melt under agitation, keeps the temperature degasification 18 minutes;
3) indium gold mixed liquor, is poured into mold at a temperature of 200 DEG C, is cooled to room temperature, eutectic composition or hypoeutectic ingredient are formed Indium billon ingot casting;
4), by ingot casting progress hot pressing rolling processing, (50 DEG C, hot rolling pass deformation rate is 5%), to remove internal porosity and crystal boundary;
5) heat treatment 3 hours, is homogenized at a temperature of 100 DEG C to the alloy cast ingot after hot pressing rolling processing using heating furnace;
6), ingot casting is cut using linear cutting equipment, realizes that thickness is thinned;
7), the ingot casting after being thinned is polished, essence throws and forms target, and anneal 10s under the conditions of 100 DEG C, obtains sample 3.
Comparative example
Comparison is " gold-germanium alloy sputtering target material and preparation method thereof " implementation application No. is " 201510568296.1 ", patent name Example 1 obtains sample 4.
Test
Sample 1-4: use by polishing, carrier concentration 1015With 1018cm-3Between N-type gallium arsenide film, successively three Vinyl chloride (analysis is pure), acetone (analysis is pure) and dehydrated alcohol are cleaned by ultrasonic each 3 minutes, remove the organic contaminant on surface.With It is respectively 10,20,30,40,50,60,70 and 80 μm of rectangular windows that the method for photoetching, which forms interval in sample surfaces, window Long and width is 250 and 200 μm, as shown in Figure 1.Sample after photoetching respectively rinses 1 point in 30% hydrochloric acid and 10% hydrofluoric acid respectively Clock to remove surface oxide layer, rinse, then is dried up with high pure nitrogen by deionized water, is packed at once equipped with indium silver-gold alloy target material Deposited metal (power 100w, sputtering time ten minutes) in magnetron sputtering apparatus.After splash-proofing sputtering metal, sample is immersed in acetone and (is divided Analyse pure) in ultrasound removing, form the figure of needs.Then mesa etch is carried out, resolution chart is isolated with ambient enviroment.Than connecing Using transmission line model method, (TLM is to measure ohmic contact resistance tradition and mature method, such as the measurement of touching resistivity Li Fengxia: TLM, electric and electronic teaching journal, the 2nd phase of volume 24).Fig. 2 is the edge pattern SEM for the electrode that spacing is 20 μm Figure, as seen from the figure, indium gold metal-semiconductor contact has excellent local edge, this is for retainer member size constancy Under the conditions of reduce source and drain spacing and improve breakdown voltage it is highly beneficial, while also be conducive to reduce device noise, better controller Part design, further promotes the optimization of device architecture.Table 1 be N-type gallium arsenide surface production ohmic contact resistance rate with move back Fiery conditional relationship, from table 1 it follows that at room temperature, the indium gold alloy electrodes prepared by magnetically controlled sputter method are in N-type arsenic Change gallium surface and form good Ohmic contact, ohmic contact resistance can be down to 5.6 × 10-7Ω·cm2, have with 4 gold germanium of sample The similar effect of target simultaneously because being needed not move through complicated short annealing process using indium silver-gold alloy target material, therefore is compared In gold-germanium alloy, good Ohmic contact can be directly formed in gallium arsenide surface using indium silver-gold alloy target material.Meanwhile for this hair The bright indium silver-gold alloy target material being related to commercial alloys target plastic property studies have shown that the elongation after fracture of indium billon is reachable 23.5-30%, and the elongation after fracture of gold-germanium alloy target is only 12.7%, therefore with the indium silver-gold alloy target material modeling of pure metal preparation Property is more preferable, can be processed into required shape according to the demand of different occasions.
The ohmic contact resistance rate and annealing conditions relationship that table 1 makes in N-type gallium arsenide surface
Sample number into spectrum Annealing temperature (DEG C) Annealing time (s) Contact resistivity (Ω cm2)
1 Room temperature 0 5.6×10-7
2 50 10 6.52×10-7
3 100 10 5.6×10-5
4 800 10 5.8×10-7

Claims (5)

1. a kind of alloy target material for forming Ohmic contact on N-type compound semiconductor materials surface, which is characterized in that including as follows Component: 2-8 wt% gold and 92-98 wt% indium.
2. a kind of a kind of alloys target for forming Ohmic contact on N-type compound semiconductor materials surface as described in claim 1 The preparation method of material, which comprises the steps of:
1), indium metal is melted using vacuum induction melting furnace, then gold nano powder is mixed into the indium metal of molten condition And it stirs evenly;
2), melt under agitation, keeps the temperature degasification 15-20 minutes;
3) indium gold mixed liquor, is poured into mold at a temperature of 180-220 DEG C, is cooled to room temperature, indium billon ingot casting is formed;
4) ingot casting, is subjected to hot pressing rolling processing, removes internal porosity and crystal boundary;
5) it is small that the alloy cast ingot after, being processed using heating furnace to hot pressing rolling homogenizes heat treatment 1-5 at a temperature of 80-120 DEG C When;
6), ingot casting is cut using linear cutting equipment;
7), the ingot casting after being thinned is polished, essence throws and forms target.
3. a kind of alloy target material for forming Ohmic contact on N-type compound semiconductor materials surface according to claim 2 Preparation method, which is characterized in that the indium metal melting condition in the step 1) are as follows: vacuum degree be 8-12 Pa vacuum In induction melting furnace, indium raw material are heated to 200-220 DEG C, after indium metal all melts, keep the temperature 30-40 minutes.
4. a kind of alloy target material for forming Ohmic contact on N-type compound semiconductor materials surface according to claim 2 Preparation method, which is characterized in that hot pressing rolling condition in the step 4) is 45-55 DEG C.
5. a kind of alloy target material for forming Ohmic contact on N-type compound semiconductor materials surface according to claim 4 Preparation method, which is characterized in that it is 3-8% that the ingot casting, which carries out hot pressing rolling pass deformation rate,.
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CN1564315A (en) * 2004-03-23 2005-01-12 中国科学院上海技术物理研究所 Device and method for measuring movability of semiconductor excess carrier and diffusion length
CN1677694A (en) * 2005-04-27 2005-10-05 中国科学院上海技术物理研究所 Gallium nitride ultraviolet detector
CN1913181A (en) * 2005-08-12 2007-02-14 璨圆光电股份有限公司 Crystal method of luminous dipolar chip and its structure
CN101232774A (en) * 2007-01-24 2008-07-30 南京汉德森科技股份有限公司 High heat conductivity ceramic base printed circuit board and method for making the same
CN101157163A (en) * 2007-11-19 2008-04-09 贵研铂业股份有限公司 A gold alloy soldering material and method of manufacture
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CN102683490A (en) * 2012-05-09 2012-09-19 上海大学 Method for preparing In heavily-doped Au/In ohmic contact electrode on surface of cadmium zinc telluride crystal
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