CN1159491A - Method for high-speed gas-phase grown diamond - Google Patents
Method for high-speed gas-phase grown diamond Download PDFInfo
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- CN1159491A CN1159491A CN 96115136 CN96115136A CN1159491A CN 1159491 A CN1159491 A CN 1159491A CN 96115136 CN96115136 CN 96115136 CN 96115136 A CN96115136 A CN 96115136A CN 1159491 A CN1159491 A CN 1159491A
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- Prior art keywords
- gas
- reaction
- phase
- grown diamond
- phase grown
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 24
- 239000010432 diamond Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 23
- 239000012495 reaction gas Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 7
- 230000004907 flux Effects 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 5
- 238000007560 sedimentation technique Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 12
- 238000000151 deposition Methods 0.000 description 7
- 239000000376 reactant Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000002787 reinforcement Effects 0.000 description 3
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 2
- 229910001573 adamantine Inorganic materials 0.000 description 2
- 230000001970 hydrokinetic effect Effects 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a high-speed gas-phase growing method of diamond. Said invention adopts a hot-wire chemical gas-phase sedimentation technique and is characterized by that its total overall reaction process is implemented in closed space, an the reaction gas is uniformly passed through reaction zone, and the gas mass flow flux is 100-200 SCCM/sq.cm, the temp. of reaction zone is kept at 2000-2600 deg.C, and the reacted gas can be discharged in good time. Said invention can quick make high-quality diamond grow up on large area.
Description
The present invention relates to the preparation of man-made diamond, provide especially with the adamantine method of heated filament heating technique high speed gas phase large area deposition.
The success of gas-phase grown diamond technology of preparing and device research has been showed attractive application prospect for people.Yet, by the prepared in laboratory technology on the problem of industrial-scale production technical change, also have many unsolved difficult problems.Wherein one of distinct issues are that quality and growth velocity standard are with satisfactory to both parties.For example, microwave plasma CVD and hot-wire chemical gas-phase deposition can reach preferable quality, but its growth velocity is more usually below 10 μ m/h.Otherwise, though the growth velocity of arc plasma jet method and flame method is higher, contain more non-diamond inclusion in its sedimentation products, be difficult to obtain qualified product.Because above various reasons, the cost of gas-phase grown diamond is also too high so far, has had a strong impact on its application.Therefore, be necessary under the prerequisite of ensuring the quality of products, to significantly improve diamond film speed, to reduce cost significantly.From the consideration of meeting the need of market, high growth velocity is again the requisite prerequisite that realizes the stable mass supply of material and the large size goods are provided.
The object of the present invention is to provide a kind of method of gas-phase grown diamond, can be on than big area, the high-quality diamond of high-speed rapid growth.
The invention provides a kind of method of high-speed gas-phase grown diamond, adopt the hot-wire chemical gas-phase deposition technology, it is characterized in that: the reaction whole process is carried out in enclosed space, and by reaction zone, the gas mass flow flux is 100-200SCCM/cm to reaction gas equably
2, reaction zone temperature remains on 2000-2600 ℃, and reaction back gas is in time discharged.
The present invention makes to put that the big area high-speed rapid growth of diamond becomes possibility owing to comprehensively adopted following technique measures before high quality.
1. reactive material is introduced the hydrokinetics reinforcement of reaction zone transport process
(1). improve the reactant gases mass rate on the unit surface.
With the reactant gases mass rate flux on the unit surface, by the 10-20SCCM/cm of common hot-wire chemical gas-phase deposition
2, bring up to 100-200SCCM/cm
2
The acceleration of reactant is sent into, and helps strengthening adamantine vapor phase growth reaction process.But, can reach this target, depend on that also can a series of reacting dynamics condition obtain solid assurance.For example, if the flow direction of reactant gases is not controlled, the quite big a part of reactant gases of then sending into does not probably enter reaction zone, flows but walk around reaction zone, directly is deflated pump and takes away.Along with the increasing of reaction gas flow, heating power must have corresponding raising thereupon, could guarantee that the active particle concentration level does not descend, and diamond film speed just may improve.If not corresponding raising of heating power or raising amount are not enough, then increase reaction gas flow, be difficult to make diamond film speed to significantly improve, even might cause its decline.At last, along with the raising of diamond film speed, resultant of reaction content will sharply increase, and its consequence is that chemical equilibrium will cause diamond film speed to descend, even poison the surfactivity point to moving in the other direction, makes the pause that reacts completely.
(2). adopt the current limliting pipeline
Exported by the reaction gas distribution device, up to the vapour deposition district, mobile all the placing in the constant section duct with reaction process of all gas carried out, and makes reactant gases many as far as possible by the high-temperature zone, fully reacts.Pipeline is made with hexagonal boron nitride or magnesium oxide material, to guarantee enough high temperature resistant and high temperature electrical insulation capabilities.Pipeline self and gas inlet seam crossing all should guarantee good air-tightness, in case reactant gases leaks midway.
2. the heated filament of gas-phase chemical reaction process is strengthened
Choose suitable heater voltage and electric current, make the temperature of heater strip remain on 2000-2600 ℃ of scope, promptly when increasing reaction gas flow, with pyrometer monitoring heater strip temperature, regulate heating current simultaneously, the hot-wire temperature is remained unchanged, thereby can keep the rate of decomposition of constant molecular hydrogen dissociation rate and carbon source material, strengthen under the parameter constant condition at heater strip, improve growth of diamond speed.
3. gas-phase chemical reaction generates the hydrokinetics reinforcement that material is derived the reaction zone transport process
0.5～1.5cm place is provided with the exhaust flared horn under sample holder, to react the gas-phase product that generates through gas exhaust duct and directly send into off-gas pump, because whole process is carried out in narrow enclosed space, help the reinforcement of realization response resultant and transport discharge, chemical equilibrium is moved to left, therefore can improve diamond film speed.
The equipment of realizing abovementioned technology comprises vacuum system, reaction chamber, part such as automatically controlled, and it is characterized in that: the entire reaction chamber is a full-closed structure, and reaction gas inlet (2) is established on the top, and perverse gas exhaust duct (9) is established in the bottom;
What be right after reaction gas inlet (2) is gas distributor (1), and its top is tower structure, interior dress 2-10 porous throttling dividing plate (3); The bottom is a tubular, and the hot wire heater of parallel array (4) is arranged on simplified bottom;
Reaction chamber is prismatic current limliting pipeline, and the boosting silk is included in wherein.
By embodiment in detail the present invention is described in detail below in conjunction with accompanying drawing
Embodiment 1
By the 14 long diameter 1mm of 170mm tungsten filaments, press the resistance heater that 10mm silk spacing constitutes, the even heating area of 100 * 100mm can be provided, flow to substrate by gas distributor through 4 layers of dividing plate and well heater.Substrate to well heater spacing is 10mm.When reaction gas flow is 20SLM, when the heater strip temperature is 2200-2600 ℃, can on the growth area of 100mm * 100mm, realizes uniform deposition, and reach the diamond film speed of 40 μ m/M.
By the 55 long diameter 1mm of 600mm tungsten filaments, press the resistance heater that 10mm silk spacing constitutes, the even heating area of 500 * 500mm can be provided, flow to substrate by gas distributor through 8 layers of dividing plate and well heater.Substrate to well heater spacing is 15mm.When reaction gas flow is 500SLM, when the heater strip temperature is 2200-2600 ℃, can on the growth area of 500mm * 500mm, realizes uniform deposition, and reach the diamond film speed of 35 μ m/M.
Claims (3)
1. the method for a high-speed gas-phase grown diamond adopts the hot-wire chemical gas-phase deposition technology, it is characterized in that: the reaction whole process is carried out in enclosed space, and by reaction zone, the gas mass flow flux is 100-200SCCM/cm to reaction gas equably
2, reaction zone temperature remains on 2000-2600 ℃, and reaction back gas is in time discharged.
2. equipment that is exclusively used in the described high-speed gas-phase grown diamond method of claim 1, comprise vacuum system, reaction chamber, part such as automatically controlled, it is characterized in that: the entire reaction chamber is totally-enclosed pipeline configuration, and reaction gas inlet (2) is established on the top, and thorn gas exhaust duct (9) is established in the bottom;
What be right after reaction gas inlet (2) is gas distributor (1), and its top is tower structure, interior dress 2-10 porous throttling dividing plate (3); The bottom is a tubular, and the hot wire heater of parallel array (4) is arranged on the bottom of cylindrical shell;
Reaction chamber is prismatic current limliting pipeline, and the boosting silk is included in wherein.
3. by the equipment of the described high-speed gas-phase grown diamond method of claim 2, it is characterized in that substrate and well heater spacing are the 5-20mm scope, distance is 5-12mm between the heater strip.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96115136 CN1159491A (en) | 1996-03-07 | 1996-03-07 | Method for high-speed gas-phase grown diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96115136 CN1159491A (en) | 1996-03-07 | 1996-03-07 | Method for high-speed gas-phase grown diamond |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1159491A true CN1159491A (en) | 1997-09-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96115136 Pending CN1159491A (en) | 1996-03-07 | 1996-03-07 | Method for high-speed gas-phase grown diamond |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1159491A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093084C (en) * | 1999-11-11 | 2002-10-23 | 袁德祎 | Method for regenerating diamond with waste material |
| CN102719804A (en) * | 2012-07-02 | 2012-10-10 | 兰州大学 | Growing device of gas inner circulation type hot wire chemical vapor deposition (CVD) diamond films |
| CN108660429A (en) * | 2018-03-23 | 2018-10-16 | 浙江工业大学 | A kind of crystal grain closs packing N-type nano-diamond film and preparation method thereof |
-
1996
- 1996-03-07 CN CN 96115136 patent/CN1159491A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093084C (en) * | 1999-11-11 | 2002-10-23 | 袁德祎 | Method for regenerating diamond with waste material |
| CN102719804A (en) * | 2012-07-02 | 2012-10-10 | 兰州大学 | Growing device of gas inner circulation type hot wire chemical vapor deposition (CVD) diamond films |
| CN102719804B (en) * | 2012-07-02 | 2014-12-10 | 兰州大学 | Growing device of gas inner circulation type hot wire chemical vapor deposition (CVD) diamond films |
| CN108660429A (en) * | 2018-03-23 | 2018-10-16 | 浙江工业大学 | A kind of crystal grain closs packing N-type nano-diamond film and preparation method thereof |
| CN108660429B (en) * | 2018-03-23 | 2020-06-23 | 浙江工业大学 | Grain-close-packed n-type nano-diamond film and preparation method thereof |
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