CN1112463C - Plasma chemical vapor deposition filing method and equipment - Google Patents
Plasma chemical vapor deposition filing method and equipment Download PDFInfo
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- CN1112463C CN1112463C CN 00128293 CN00128293A CN1112463C CN 1112463 C CN1112463 C CN 1112463C CN 00128293 CN00128293 CN 00128293 CN 00128293 A CN00128293 A CN 00128293A CN 1112463 C CN1112463 C CN 1112463C
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- arc
- plasma field
- heater
- ionization
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- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 16
- 239000007921 spray Substances 0.000 claims abstract description 7
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 6
- 238000010891 electric arc Methods 0.000 claims abstract description 3
- 230000000694 effects Effects 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 22
- 238000000576 coating method Methods 0.000 abstract description 14
- 239000011248 coating agent Substances 0.000 description 13
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 8
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 208000005168 Intussusception Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Physical Vapour Deposition (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
本发明等离子化学气相沉积镀膜方法和设备包括：传统的可抽成真空的炉体；将汽化的、含有金属氯化物的和其它工作气体通入所述真空炉体内的装置；放置在真空炉体中的被镀工件与电极阴极相连，将炉体与阳极相连，阳极接地，阴极施加负电压，将电压升高到一定程度后，阴、阳级之间产生辉光等离子场；在所述炉内设置一个能喷出等离子炬的电弧喷枪，电弧喷枪喷出的等离子炬直接进入到辉光等离子场中。
The plasma chemical vapor deposition coating method and equipment of the present invention include: a traditional furnace body that can be evacuated; a device for passing vaporized, metal chloride-containing and other working gases into the vacuum furnace body; placed in the vacuum furnace body The workpiece to be plated is connected to the cathode of the electrode, the furnace body is connected to the anode, the anode is grounded, and the cathode is applied with a negative voltage. After the voltage is raised to a certain level, a glow plasma field is generated between the cathode and the anode; in the furnace An electric arc spray gun capable of ejecting a plasma torch is arranged inside, and the plasma torch ejected by the arc spray gun directly enters the glow plasma field.
Description
The present invention relates to a kind of new-type, with the method and apparatus of Plasma Enhanced Chemical Vapor Deposition (PECVD) at the workpiece surface plated film, belong to the plasma chemical vapor deposition process technical field.
Has been known to the public with Plasma Enhanced Chemical Vapor Deposition (PECVD) in the technology of workpiece or substrate surface plating many types coating.With the titanium-nitride is example, and the technical equipment that generally adopts is now: in the vacuum oven of a sealing, workpiece to be plated is linked to each other with electrode cathode, plus earth, negative electrode applies negative voltage, when negative voltage is raised to a certain degree, produces the glow plasma field between the cathode and anode.Temperature in the stove is remained on about 500 degree, feed working gass such as the muriatic volatilization steam of titaniferous and nitrogen, hydrogen, argon gas in the stove in proportion simultaneously, under the acting in conjunction of high temperature and argon-arc plasma field, all gases molecular breakdown, ionization, generation chemical reaction, formation of deposits titanium nitride coating on workpiece surface.This technology those skilled in the art is for this reason known.But this technology has following shortcoming:
1, the ionization level of most metal chlorides in the glow plasma field is very low, and for example when 500-600 spends, the ionization level of titanium tetrachloride in the glow plasma field is lower than percent 10.The very low meeting of ionization level causes the cl content height in the coating, microtexture, mechanical property and poor corrosion resistance, and at the bottom of the coating sedimentation rate.
2, owing to the working temperature of stove domestic demand 500 degree, the workpiece that many non-refractory materials are made can not be suitable for this method;
3, above-mentioned low ionization level and high temperature require also to make integral device more complicated, uneconomical.
The present invention makes for overcoming above-mentioned the deficiencies in the prior art exactly.
The object of the invention provide a kind of can be at normal temperatures, realize that the Plasma Enhanced Chemical Vapor Deposition (PECVD) of high ionization level prepares the technological method and the equipment of coating.
Further purpose of the present invention provide a kind of have high ionization level, simple, the good economy performance of equipment, and sedimentation rate height can be applicable to that the made workpiece of different temperature-resistant materials carries out technological method and equipment that Plasma Enhanced Chemical Vapor Deposition (PECVD) prepares coating.
Another object of the present invention provide a kind of have high ionization level, the equipment simple economy is good and the efficient height of metallizing oxide compound, metal nitride, metallic carbide, be suitable for the method and apparatus of the workpiece that the various materials of plating make.
The present invention's summary:
Plasma Chemical vapor deposition filing method of the present invention comprises: one traditional can evacuated body of heater; Traditional that will vaporize, contain metal chloride feed the intravital device of described vacuum oven with other working gas; The workpiece to be plated that is placed in the vacuum furnace body is linked to each other with electrode cathode, body of heater is linked to each other with anode, plus earth, negative electrode applies negative voltage, bring the voltage up to a certain degree after, produce the glow plasma field between the yin, yang level; Make the described gas that feeds in the stove be arranged on arc pistol in the vacuum oven, that can spray plasmatorch by one, described spray gun forms an arc plasma field, the energy that is produced by electric arc forces the gas molecule ionization of passing through, and the plasmatorch of arc pistol ejection directly enters described glow plasma field; Through ion that the ionization of arc plasma field goes out and ionization goes out after the secondary ionization in described glow plasma field ion generation chemical reaction and in electrical forces effect deposit on the workpiece to be plated surface.
Plasma Chemical vapor deposition filing equipment of the present invention comprises: one traditional can evacuated body of heater; Traditional that will vaporize, contain metal chloride feed the intravital device of described vacuum oven with other working gas; The workpiece to be plated that is placed in the vacuum furnace body links to each other with electrode cathode, body of heater is linked to each other with anode, plus earth, negative electrode applies negative voltage, bring the voltage up to a certain degree after, produce the glow plasma field between the yin, yang level; An arc pistol is set in the described stove, the ionization of gas that arc pistol will pass through, the plasmatorch of arc pistol ejection directly is injected in the described glow plasma field.
Present device further comprises, traditional arc power and circulating water cooling device that described arc pistol uses; Described body of heater links to each other with the cold-trap device of getting rid of residue.
The present invention is further described below by one embodiment of the present of invention.
Accompanying drawing 1 be existing, at traditional plasma Chemical vapor deposition filing equipment of workpiece surface titanium-nitride;
Accompanying drawing 2 is present devices;
Among Fig. 1, the 1st, the sealing body of heater of vacuum-pumping; The 2nd, to the well heater of body of heater internal heating; The 3rd, titanium tetrachloride gases is provided in body of heater and comprises the device of working gass such as hydrogen, nitrogen; The 4th, the cold-trap device of traditional discharging residue; The 5th, workpiece to be plated or negative electrode loading frame; The 6th, power supply, its anode links to each other with body of heater, negative electrode links to each other with workpiece.When being in certain vacuum degree, voltage across poles in the body of heater chamber when enough high, form the glow plasma field between the cathode and anode.This moment as well heater with the body of heater inner chamber heat spend to 500 about, feed titanium tetrachloride gases and other working gas by a certain percentage, under the effect of glow plasma field, concurrent biochemical reaction is decomposed in above-mentioned gas generation ionization, forms titanium nitride coating in electrical forces effect deposit at the workpiece surface negative electrode.Technology shown in Figure 1 and Apparatus and method for are well known to those skilled in the art.
Fig. 2 is the present device synoptic diagram, among Fig. 2, and the 1st, the sealing body of heater of vacuum-pumping; The 4th, the cold-trap device of discharging residue; The 5th, workpiece to be plated or negative electrode loading frame; The 6th, power supply, its anode links to each other with body of heater, negative electrode links to each other with workpiece.When being in certain vacuum degree, voltage of supply in the body of heater chamber when enough high, form the glow plasma field in the body of heater chamber between cathode and anode.The 8th, arc pistol, the 9th, the arc power of arc pistol, the 10th, the circulating water cooling device of arc pistol 8; The 3rd, arc pistol 8 provides the device of titanium tetrachloride gases and working gas in body of heater; The 11st, gas enters the inlet of arc pistol 8, and the 12nd, the outlet of arc pistol 8 ejection plasmatorchs, the plasmatorch of 13 expression arc pistol ejections.Working process is, when being in the certain vacuum degree in the body of heater chamber, when power supply 6 voltages are enough high, forming the glow plasma field in the body of heater chamber.The arc power 9 of arc pistol 8 is opened, install 3 simultaneously and pass through arc pistol 8 gas inletes 11 to the spray gun air feed, arc pistol 8 forces under the energy that arc power 9 provides and enters gas starting the arc ionization, and directly is injected to the glow plasma field that has formed in the body of heater from exporting 12.Since enter gas at first arc pistol 8 in formation the arc plasma field in by ionization, from export 12 directly enter plasma aura field after, the ion of ionization can keep the ionization state, can not carried out the secondary ionization by the gas of ionization, thereby has improved ionization level greatly.By the ion generation chemical reaction of ionization, and on workpiece to be plated 5, form titanium nitride coating in the electric field action power deposit of glow plasma field.Employed arc pistol 8 is the currently available productss that exist in the market, and it needs arc power when using, and the recirculated cooling water passage is arranged on the product, and gas admission port and outlet are arranged.The characteristics of this arc pistol are to eject plasmatorch in the exit.
Below introduce one with the inventive method and equipment result to the workpiece titanium-nitride:
Processing parameter is as follows:
Air pressure 300-500Pa, voltage 900V, electric current 15A, frequency 100Hz (pulse direct current plasma aura field); Voltage 20-30V, electric current 90-110A (arc plasma field), in the vacuum oven temperature 40-60 ℃, workpiece temperature 50-80 ℃, (do not heat, there is certain intensification effect arc plasma field and glow plasma field), working gas is N
2, H
2, Ar, TiCL
4Input by a certain percentage, workpiece to be plated is the rapid steel sample.
The TiN coating that obtains at workpiece surface under these conditions, through scanning electronic microscope and X-ray energy spectrometer assay determination, the cl content in the coating levels off to zero (content is lower than the sensitivity of instrument).And the cl content average out to 2% in the TiN coating that obtains with legacy equipment.The result that chlorinity in the TiN coating reduces significantly illustrates that also the inventive method and equipment can increase substantially the ionization level of working gas.
The present invention is owing to adopted arc pistol in traditional plasma Chemical vapor deposition filing equipment, thereby make arc plasma field and glow plasma field form intussusception, this measure has not only improved ionization level greatly, has improved production efficiency, and has saved heating unit.Especially, can not carry out plasma Chemical vapor deposition filing, then can now with traditional method for some workpiece of can not high temperature material making.Enlarged the scope of suitable workpiece thus again.Obviously the inventive method and equipment are applicable to that also multiple material workpiece carries out the plasma Chemical vapor deposition filing of dissimilar coating.
This shows that the inventive method and equipment have been finished the object of the invention, its excellent effect is tangible.Those skilled in the art can understand and implement the present invention fully according to its due knowledge.The non-creativeness of being done under the present invention conceives inspiration that does not break away from essence design of the present invention changes, and also belongs to protection domain of the present invention.Protection domain of the present invention is defined by the claims.
Claims (3)
1, a kind of plasma Chemical vapor deposition filing method comprises: one traditional can evacuated body of heater; Traditional that will vaporize, contain metal chloride feed the intravital device of described vacuum oven with other working gas; The workpiece to be plated that is placed in the vacuum furnace body is linked to each other with electrode cathode, body of heater is linked to each other with anode, plus earth, negative electrode applies negative voltage, bring the voltage up to a certain degree after, produce the glow plasma field between the yin, yang level; It is characterized in that: be under the normal temperature situation at vacuum oven, make the described gas that feeds in the stove be arranged on arc pistol in the vacuum oven, that can spray plasmatorch by one, described spray gun forms an arc plasma field, the energy that is produced by electric arc forces the gas molecule ionization of passing through, and the plasmatorch of arc pistol ejection directly enters described glow plasma field; Through ion that the ionization of arc plasma field goes out and ionization goes out after the secondary ionization in described glow plasma field ion generation chemical reaction and in electrical forces effect deposit on the workpiece to be plated surface.
2, a kind of plasma Chemical vapor deposition filing equipment comprises: one traditional can evacuated body of heater; Traditional that will vaporize, contain metal chloride feed the intravital device of described vacuum oven with other working gas; The workpiece to be plated that is placed in the vacuum furnace body links to each other with electrode cathode, body of heater is linked to each other with anode, plus earth, negative electrode applies negative voltage, bring the voltage up to a certain degree after, produce the glow plasma field between the yin, yang level; It is characterized in that: at vacuum oven is under the normal temperature situation, and an arc pistol is set in the stove, the ionization of gas that arc pistol will pass through, and the plasmatorch of arc pistol ejection directly is injected in the described glow plasma field.
3, by the described equipment of claim 2, it is characterized in that: arc pistol uses traditional arc power and circulating water cooling device; Described sealing body of heater links to each other with the cold-trap device of getting rid of residue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00128293 CN1112463C (en) | 2000-12-15 | 2000-12-15 | Plasma chemical vapor deposition filing method and equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00128293 CN1112463C (en) | 2000-12-15 | 2000-12-15 | Plasma chemical vapor deposition filing method and equipment |
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| Publication Number | Publication Date |
|---|---|
| CN1308147A CN1308147A (en) | 2001-08-15 |
| CN1112463C true CN1112463C (en) | 2003-06-25 |
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| CN 00128293 Expired - Fee Related CN1112463C (en) | 2000-12-15 | 2000-12-15 | Plasma chemical vapor deposition filing method and equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4233085B2 (en) * | 2003-02-17 | 2009-03-04 | 日本碍子株式会社 | Thin film manufacturing method and apparatus |
| CN106211763B (en) * | 2014-03-25 | 2019-08-27 | 住友金属矿山株式会社 | Coated solder material and its manufacturing method |
| TWI846040B (en) * | 2015-08-07 | 2024-06-21 | 加拿大商高純石英 矽資源公司 | Silica to high purity silicon production apparatus and process |
| CN110672667B (en) * | 2019-10-17 | 2021-02-26 | 北京航空航天大学 | A dynamic piezoresistive probe for measuring plasma deposition |
| CN111020535B (en) * | 2020-01-10 | 2021-12-17 | 佛山市思博睿科技有限公司 | Preparation method of plasma chemical vapor deposition nano-film of cell counting plate |
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