CN1916233B - Organometallic compound supply container - Google Patents
Organometallic compound supply container Download PDFInfo
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- CN1916233B CN1916233B CN2006101108485A CN200610110848A CN1916233B CN 1916233 B CN1916233 B CN 1916233B CN 2006101108485 A CN2006101108485 A CN 2006101108485A CN 200610110848 A CN200610110848 A CN 200610110848A CN 1916233 B CN1916233 B CN 1916233B
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- organometallic compound
- container
- carrier gas
- carrier
- supply container
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Abstract
一种有机金属化合物供给容器，在容器上部配设载气导入管的前端部，底部配设载气导出管的前端部，且在该容器内填充载体担载有机金属化合物而构成，该载体担载有机金属化合物是在相对于有机金属化合物惰性的载体上被覆常温下固体的有机金属化合物而构成，该有机金属化合物供给容器的特征在于，载气导入管的前端部相对于水平方向向斜下方倾斜20～50°而配设。由此提供能够获得具有一定的重复性的有机金属化合物的蒸发量，增加载气流量并增加有机金属化合物的气化量时，能够减少填充的有机金属化合物的使用率的降低的有机金属化合物供给容器。
An organometallic compound supply container is provided with a front end of a carrier gas introduction pipe on the upper part of the container, and a front end of a carrier gas outlet pipe on the bottom, and the container is filled with a carrier carrying an organometallic compound. The organometallic compound-carried carrier is formed by coating an organometallic compound that is solid at normal temperature on a carrier that is inert to the organometallic compound. The organometallic compound supply container is characterized in that the front end of the carrier gas introduction pipe is inclined downward with respect to the horizontal direction. It is installed at an inclination of 20-50°. This provides an organometallic compound supply capable of obtaining a certain reproducible vaporization amount of the organometallic compound, increasing the flow rate of the carrier gas and increasing the vaporization amount of the organometallic compound, and reducing the decrease in the utilization rate of the organometallic compound to be filled. container.
Description
Technical field
The present invention relates to organic metal compound supply container.Relate in particular to and fill the organic metal compound supply container that the supported carrier organometallic compound forms, this supported carrier organometallic compound is overlayed on the solid organometallic compound to have on the inert carrier with respect to organometallic compound to form at normal temperatures.
Background technology
Organometallic compound is in the electronic industry purposes, and for example the raw material as compound semiconductor uses.When in electronic industry, using organometallic compound, make carrier gas such as hydrogen mobile contiguously usually, import in the epitaxially growing equipment etc. as the saturated vapo(u)r of organometallic compound and use with organometallic compound.
For solid organometallic compound under the normal temperature (room temperature), there is following shortcoming: even be blown into the carrier gas different with liquid, also form the stream that carrier gas is passed through in the solid organometallic compound of lamination, perhaps the solid organometallic compound that becomes small particle size because of gasification is stacked into container bottom, its result can't obtain solid organometallic compound and contact with the sufficient of carrier gas, thereby can't supply with the organometallic compound of stable concentration to epitaxially growing equipment.
For solid state organometallic compound under this normal temperature, container as the steam output of the organometallic compound that can obtain to have certain repeatability, known have: the container upper vertical set the leading section of carrier gas ingress pipe, the bottom sets the leading section of carrier gas delivery line, and the vapor phase growth organic metal compound supply container of filling the supported carrier organometallic compound in the container and constituting, this supported carrier organometallic compound are to constitute (spy opens flat 1-265511 communique) have lining organometallic compound on the inert carrier with respect to organometallic compound.
But, there is following problems in the supply container of putting down in writing in the Te Kaiping 1-265511 communique: although can obtain to have the steam output of the organometallic compound of certain repeatability, if but in order to improve the efficient of vapor phase growth, increase carrier gas flux and increase the amount of vaporization of organometallic compound, then the rate of utilization of the organometallic compound of Tian Chonging reduces, promptly, can not obtain the time point that certain density organometallic compound contains gas becoming, residual organometallic compound increases in the supply container.Have, take out organometallic compound residual in the supply container etc., clean container inside utilizes container again.
Summary of the invention
The object of the present invention is to provide a kind of organic metal compound supply container, it can obtain to have the steam output of the organometallic compound of certain repeatability, when increasing carrier gas flux and increasing the amount of vaporization of organometallic compound, can reduce the reduction of rate of utilization of the organometallic compound of filling.
The present inventor is in order to solve found that described problem studies with keen determination: employing will be located at container top to tilt 20～50 ° the leading section of carrier gas ingress pipe of oblique below with respect to horizontal direction, the bottom sets the container of the leading section of carrier gas delivery line, in container, fill the supported carrier organometallic compound, this supported carrier organometallic compound is to constitute have solid organometallic compound under the normal temperature that is covered on the inert carrier with respect to organometallic compound, import carrier gas from the leading section of carrier gas ingress pipe, derive the carrier gas of the organometallic compound that contains gasification from the carrier gas delivery line, can obtain to have the steam output of the organometallic compound of certain repeatability thus, when increasing carrier gas flux and increasing the amount of vaporization of organometallic compound, can reduce the reduction of rate of utilization of the organometallic compound of filling, thereby realize the present invention.
Promptly, the present invention is the leading section that sets the carrier gas ingress pipe on container top, the bottom sets the leading section of carrier gas delivery line, and in this container, fill the supported carrier organometallic compound and constitute, this supported carrier organometallic compound is to constitute have solid organometallic compound under the normal temperature that is covered on the inert carrier with respect to organometallic compound, this organic metal compound supply container is characterised in that the leading section of carrier gas ingress pipe sets to 20～50 ° of oblique below inclinations with respect to horizontal direction.
By adopting the organic metal compound supply container that is filled with the supported carrier organometallic compound of the present invention, this supported carrier organometallic compound is to constitute have solid organometallic compound under the normal temperature that is covered on the inert carrier with respect to organometallic compound, can obtain to have the steam output of the organometallic compound of certain repeatability, when increasing carrier gas flux and increasing the amount of vaporization of organometallic compound, can reduce the reduction of rate of utilization of the organometallic compound of filling.
Description of drawings
Fig. 1 is the diagrammatic cross-section of an embodiment of organic metal compound supply container of the present invention;
Fig. 2 is the diagrammatic cross-section of the configuration of overlooking direction of the leading section of expression carrier gas ingress pipe;
Fig. 3 is the figure of example of structure of the leading section of expression carrier gas ingress pipe;
Fig. 4 is the diagrammatic cross-section of organic metal compound supply container in the past.
Among the figure, the 1-container; 2-carrier gas ingress pipe; The leading section of 3-carrier gas ingress pipe; 4-carrier gas delivery line; The leading section of 5-carrier gas delivery line; 6-supported carrier organometallic compound; The top board of 7-container.
Embodiment
Organometallic compound of the present invention at room temperature is a solid, being used in vapor phase growth uses etc., specifically can exemplify: indium compounds such as trimethyl indium, dimethyl chlorination indium, cyclopentadienyl indium, trimethyl indium trimethylammonium arsine affixture, trimethyl indium trimethyl-phosphine affixture, zn cpdss such as ethyl zinc iodide, ethyl cyclopentadienyl zinc, cyclopentadienyl zinc, aluminum compounds such as methylaluminum dichloride, gallium compounds such as methyl dichloro gallium, dimethyl chlorination gallium, dimethyl gallium bromide, bis-cyclopentadienyl magnesium etc.
In addition, has the inert carrier as what support these organometallic compounds with respect to organometallic compound, can use ceramic-like such as aluminum oxide, silicon-dioxide, mullite (mullite), vitreous carbon, graphite, potassium titanate, quartz, silicon nitride, boron nitride, silicon carbide, metal species such as stainless steel, aluminium, nickel, tungsten, fluoro-resin, glass etc.
The shape of carrier is not particularly limited, and can use different shapes such as indefinite shape, spherical, fibrous, netted, coiled type, pipe shape.
The preferred big specific surface area of carrier, carrier surface be than slick surface, preferably has fine concavo-convex about about 100～2000 μ m, and perhaps carrier self has a plurality of pores (space).As this carrier, can exemplify alumina balls, Raschig ring, helipack (ヘ リ パ Star Network), Dixon filler (デ イ Network ソ Application パ Star キ Application), stainless steel sintered component, glass wool etc.
By the method for supported carrier organometallic compound, can adopt the general in the past method of implementing.For example can adopt following method: in advance by weight placement carrier and organometallic compound, then its heating is made the organometallic compound fusion in container, rotation is afterwards stirred and refrigerative method gradually; Make placement carrier in the organometallic compound fused process in heating, take out unnecessary fusion organometallic compound then, afterwards the refrigerative method.
When supporting, the most important thing is to remove in advance the oxygen that contains in the carrier or hygroscopic water, other volatile impunty.If carrier surface exists oxygen or moisture etc., then organometallic compound can go bad or be contaminated, thus when being used for using as vapor phase growth, the quality of the film that obtains of infringement not only, and can't accomplish stable supplying as the raw material of purpose of the present invention.For fear of this unfavorable condition, the suggestion carrier heats and carries out vacuum outgas in advance under the temperature of the scope of allowing of its material, then by inert gas replacement space parts such as nitrogen or argons.
The organometallic compound that supports on the carrier with respect to carrier 100 weight parts, is approximately 10～100 weight parts usually, the scope of preferably approximately 20～70 weight parts.When about 10 weight parts are following and since occupy vessel volume organometallic compound amount seldom, so must increase container to more than the necessary size, therefore and uneconomical.In addition, when supporting above about 100 weight parts, than situation about not supporting, the surface-area of the organometallic compound corresponding with packed space does not reach the size of the degree of expectation, so possibly can't fully obtain the effect as purpose of the present invention.
Fig. 1 is the diagrammatic cross-section of an embodiment of organic metal compound supply container of the present invention.Container 1 adopts usually has the structure cylindraceous of forniciform bottom.Carrier gas ingress pipe 2 and carrier gas delivery line 4 are installed on the top of container 1, the leading section 3 of carrier gas ingress pipe with respect to horizontal direction to oblique below tilt about 20～50 °, 25～45 ° of preferably approximatelies and set.The leading section 5 of carrier gas delivery line is provided in the bottom of container.Be filled with organometallic compound 6 at internal tank by supported carrier.Fig. 4 is the diagrammatic cross-section of organic metal compound supply container in the past, supply container of the present invention is than the supply container of in the past the leading section that vertically is equipped with the carrier gas ingress pipe 3, and difference is about 20～50 ° of leading sections 3 that set the carrier gas ingress pipe.Have again, be provided with the dispensing port (not shown) of organometallic compound and carrier or supported carrier organometallic compound in the container 1.
Carrier gas ingress pipe 2 and carrier gas delivery line 4 are installed in the top of container in Fig. 1, if but the leading section 3 of carrier gas ingress pipe is provided in the top of container, and the leading section 5 of carrier gas delivery line is provided in the bottom of container, and the sidepiece that then is installed in container is also harmless.
The leading section 3 of carrier gas ingress pipe preferably tilts about 20～50 ° with respect to horizontal direction to oblique below, and from away from the position of the central shaft of container with respect to the sidewall slope of container and set.
Fig. 2 is the diagrammatic cross-section of the configuration of overlooking direction of the leading section of expression carrier gas ingress pipe.Carrier gas ingress pipe 2 is equipped on the position away from the central shaft of cylindrical vessel, and its leading section 3 is with respect to the sidewall slope of container and set.Dispose according to this, circle round from the carrier gas formation of leading section and flow and flow (schematically being represented by arrow among the figure), bias current disappears.
Fig. 3 is the figure of example of structure of the leading section of expression carrier gas ingress pipe.(A) in, the peristome of the part of the top board 7 of container tilts about 20～50 ° to constitute leading section to oblique below with respect to horizontal direction.(B) in,, constitute leading section setting on the top board 7 with respect to horizontal direction about 20～50 ° pipe arrangement that tilts below tiltedly.
The supported carrier organometallic compound is filled into the loading level in the container, and the bottom with the leading section that is lower than the carrier gas ingress pipe is a target usually, but during by the supported carrier organometallic compound, should be about 30～70 volume % of container in container.
Represented that the bottom is forniciform container, but be not particularly limited, also can use the coniform container of Denging in this.From easness of making and the angle consideration that can stablize and supply with expeditiously certain density gas, the preferred container that adopts with forniciform bottom.
The leading section 5 of the bottom of container and carrier gas delivery line be spaced apart about 2～15mm, preferably approximately 2～10mm, further preferred 2～5mm.If greater than about 15mm, then because the reduction of the rate of utilization of organometallic compound is therefore not preferred.
Be filled be supported on carrier by above-mentioned method the supply container 1 of organometallic compound by conveyance to the field of employment, carrier gas delivery line 4 is connected with (not shown) such as epitaxially growing equipments, in addition, carrier gas ingress pipe 2 is connected with the supply source of carrier gas such as hydrogen.Supply container is remained certain temperature, supply with carrier gas, the top of carrier gas while the gap of passing the supported carrier organometallic compound from container is moved to the bottom, make the carrier gas that contains certain density organometallic compound under this temperature supply to epitaxially growing equipment etc. thus through carrier gas delivery line 4.Thus, obtain to have the steam output of the organometallic compound of certain repeatability, increasing carrier gas flux and increasing under the situation of amount of vaporization of organometallic compound, also can reduce the reduction of rate of utilization of the organometallic compound of filling.
[embodiment]
Below, in an embodiment the present invention is at length described, but the present invention is not limited to these embodiment.
Adopted following container as organic metal compound supply container.
(container A)
Container A is the stainless steel container made (forniciform bottom) of internal volume 800ml, be with Fig. 1, Fig. 2 and Fig. 3 (A) in the identical structure of structure of expression schematically, be equipped with the dispensing port of carrier gas ingress pipe 2, carrier gas delivery line 4, carrier and organometallic compound on the top board of container.Shown in Fig. 3 (A), the leading section of carrier gas ingress pipe is that the peristome of the part of container top board 7 is constituted to 30 ° of oblique below inclinations with respect to horizontal direction.In addition, as shown in Figure 2, carrier gas ingress pipe 2 is provided in the position away from the central shaft 24mm of cylindrical vessel, and its leading section 3 is with respect to the sidewall slope of container and set.In addition, the leading section 5 of the bottom of container and carrier gas delivery line is spaced apart 3mm.
(container B)
Container B be except the leading section of carrier gas ingress pipe as illustrated in fig. 4 with respect to the container top board towards vertical direction, the container identical with container A.
To in the container and after conduit carries out nitrogen replacement, under nitrogen atmosphere, in container, filled as carrier from dispensing port and to have carried out vacuum outgas, space part to have been carried out alumina balls 435g and the trimethyl indium 300g of the about 4mm Φ behind the nitrogen replacement.Container after filling is heated to more than the fusing point of trimethyl indium, makes the trimethyl indium fusion, the container rotation is cooled off gradually, thereby trimethyl indium is solidificated in the surface of the alumina balls of carrier, support thus.
(supply of organometallic compound)
Hydrogen cylinder, flow rate control device, the organic metal compound supply container that is filled with above-mentioned supported carrier organometallic compound, gas concentration meter, trimethyl indium collection are connected in this order with deep cooling collector, pressure control device and vacuum pump.
Supply container is rendered in the thermostatic bath, remains on 25 ℃.Adopted エ ピ ソ Application densitometer (ト one マ ス ス ワ Application サ イ エ Application テ イ Off イ Star Network イ Network イ Star プ メ Application ト society system) as the gas concentration meter.
Experiment 1: for the container A that is filled with the supported carrier organometallic compound, with 900ml/ branch (normal atmosphere conversion) hydrogen supply, make the trimethyl indium gasification, decided trimethyl indium concentration by the gas concentration instrumentation from the carrier gas ingress pipe.
Experiment 2: in addition,, with 900ml/ branch (normal atmosphere conversion) hydrogen supply, measured trimethyl indium concentration equally from the carrier gas ingress pipe for the container B that is filled with the supported carrier organometallic compound.
Experiment 3: in addition,, with 600ml/ branch (normal atmosphere conversion) hydrogen supply, measured trimethyl indium concentration equally from the carrier gas ingress pipe for the container B that is filled with the supported carrier organometallic compound.
Obtain the ratio (is benchmark to test 1) of their rate of utilization (obtaining the ratio of the gross weight of the trimethyl indium that gasifies during the certain density trimethyl indium gas) with respect to the trimethyl indium loading level of in container, filling.The results are shown in table 1.
[table 1]
| Experiment No. | Use container | The flow of carrier gas (ml/ branch) | The ratio of rate of utilization |
| 1 | A | 900 | 1.0 |
| 2 | B | 900 | 0.82 |
| 3 | B | 600 | 1.1 |
As above-mentioned, when using container (B) in the past, if then rate of utilization reduction of hydrogen flowing quantity increase, but the container of the application of the invention (A), even increase hydrogen flowing quantity, the situation than using container in the past also can improve rate of utilization.
Claims (4)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005-236411 | 2005-08-17 | ||
| JP2005236411A JP4710481B2 (en) | 2005-08-17 | 2005-08-17 | Organometallic compound supply container |
| JP2005236411 | 2005-08-17 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1916233A CN1916233A (en) | 2007-02-21 |
| CN1916233B true CN1916233B (en) | 2010-11-03 |
Family
ID=37737296
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2006101108485A Expired - Fee Related CN1916233B (en) | 2005-08-17 | 2006-08-15 | Organometallic compound supply container |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP4710481B2 (en) |
| CN (1) | CN1916233B (en) |
| TW (1) | TW200720472A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12369336B2 (en) * | 2020-03-02 | 2025-07-22 | Taiwan Semiconductor Manufacturing Co., Ltd. | Method and system for forming metal-insulator-metal capacitors |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102075925B1 (en) | 2016-12-07 | 2020-02-12 | 한국생산기술연구원 | Mold coating agents for titanium alloy castings, mold for titanium alloy casings using the same and manufacturing method thereof |
| CN111172513A (en) * | 2020-03-09 | 2020-05-19 | 江苏南大光电材料股份有限公司 | Container for packaging solid high-purity metal organic compound and application thereof |
| US12410514B2 (en) | 2020-12-04 | 2025-09-09 | Kojundo Chemical Laboratory Co., Ltd. | Vapor deposition source material used in production of film containing indium and one or more of the other metals, and the method of producing film containing indium and one or more of the other metals |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542918A (en) * | 2003-05-01 | 2004-11-03 | 日本派欧尼株式会社 | vaporizer |
| CN2716285Y (en) * | 2004-07-07 | 2005-08-10 | 中国航空工业第一集团公司北京航空制造工程研究所 | Precursor automatic feeding device for chemical vapor codeposition and infiltration |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2651530B2 (en) * | 1988-04-15 | 1997-09-10 | 住友化学工業株式会社 | Organometallic compound supply equipment for vapor phase growth |
| JPH0726365Y2 (en) * | 1990-01-08 | 1995-06-14 | 大日本スクリーン製造株式会社 | Chemical liquid vaporizer for vapor phase surface treatment equipment |
| JP3335492B2 (en) * | 1994-12-28 | 2002-10-15 | 三菱電機株式会社 | Thin film deposition equipment |
| JP2964313B2 (en) * | 1995-03-09 | 1999-10-18 | 信越化学工業株式会社 | Solid organometallic compound supply apparatus and method for producing the same |
| JPH1067594A (en) * | 1996-08-26 | 1998-03-10 | Sony Corp | Metal organic chemical vapor deposition equipment |
| JPH11111644A (en) * | 1997-09-30 | 1999-04-23 | Japan Pionics Co Ltd | Vaporization supply device |
| JP2000017438A (en) * | 1998-06-30 | 2000-01-18 | Japan Pionics Co Ltd | Vaporizer and vapor supply method |
| DE60106675T2 (en) * | 2000-05-31 | 2005-12-01 | Shipley Co., L.L.C., Marlborough | Evaporator |
-
2005
- 2005-08-17 JP JP2005236411A patent/JP4710481B2/en not_active Expired - Fee Related
-
2006
- 2006-08-09 TW TW095129232A patent/TW200720472A/en not_active IP Right Cessation
- 2006-08-15 CN CN2006101108485A patent/CN1916233B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542918A (en) * | 2003-05-01 | 2004-11-03 | 日本派欧尼株式会社 | vaporizer |
| CN2716285Y (en) * | 2004-07-07 | 2005-08-10 | 中国航空工业第一集团公司北京航空制造工程研究所 | Precursor automatic feeding device for chemical vapor codeposition and infiltration |
Non-Patent Citations (1)
| Title |
|---|
| JP特开平6-20951A 1994.01.28 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12369336B2 (en) * | 2020-03-02 | 2025-07-22 | Taiwan Semiconductor Manufacturing Co., Ltd. | Method and system for forming metal-insulator-metal capacitors |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI379018B (en) | 2012-12-11 |
| TW200720472A (en) | 2007-06-01 |
| CN1916233A (en) | 2007-02-21 |
| JP2007053186A (en) | 2007-03-01 |
| JP4710481B2 (en) | 2011-06-29 |
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