CN106835065B - A kind of Nano diamond silane surface vacuum pyrolysis depositing device - Google Patents
A kind of Nano diamond silane surface vacuum pyrolysis depositing device Download PDFInfo
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- CN106835065B CN106835065B CN201610900669.5A CN201610900669A CN106835065B CN 106835065 B CN106835065 B CN 106835065B CN 201610900669 A CN201610900669 A CN 201610900669A CN 106835065 B CN106835065 B CN 106835065B
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4417—Methods specially adapted for coating powder
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Abstract
A kind of Nano diamond silane surface vacuum pyrolysis depositing device, comprising: mechanical pump (1), diffusion pump (2), four-way valve (3), vacuum tube furnace (4), quartz ampoule (5), objective table (7), silane air inlet (8), argon inlet mouth (9), flowmeter (10), compound vacuum gauge (11), vent valve (12).Nano diamond surface impurity functional group under high vacuum state is pyrolyzed absorption, and silane gas is fully infiltrated between Nano diamond powder at room temperature, forms unimolecule with Nano diamond surface dangling bond or polymolecular is saturated adsorption layer, disperse is in Nano diamond surface.Subsequent adsorbate inert gas is pyrolyzed in situ, and Nano diamond surface forms atom level silicon cladding.The purification that the present invention realizes Nano diamond saves problem, can solve that purchase ALD plating equipment is expensive, and coating technology difficulty is big, at high cost, low efficiency and the problem of Nano diamond high-volume Si atom plating industrialization.
Description
Technical field
This application involves PDC cutter material manufacturing field, in particular to a kind of Nano diamond silane surface vacuum pyrolysis
Depositing device.
Background technique
Current Nano diamond employed both at home and abroad is mostly prepared by Detonation Process.Nano diamond not only has diamond
General characteristic, while there are also the small-size effect of nano material and the nanometer of great specific surface, especially detonation synthesis
Diamond contains more dislocation and distortion of lattice, therefore Nano diamond made from Detonation Process has very high surface-active,
Its adsorption has a large amount of oxygen-containing functional groups, mainly there is hydroxyl, carboxyl, carbonyl, ether, ester group and some nitrogenous groups.
So the purifying problem on Nano diamond surface and purified preservation problem become Nano diamond downstream application needs
The key technical problem of solution.
To solve the above problems, the purified treatment Nano diamond first under high vacuum state, makes the big of its adsorption
Measure oxygen-containing, the nitrogenous, desorption of functional group containing Cl.Silane gas is imported after being cooled to room temperature into reaction chamber, is sufficiently seeped under negative pressure
Enter between the Nano diamond powder of accumulation.Part precursor molecule reacted with Nano diamond surface dangling bond to be formed unimolecule or
Polymolecular be saturated adsorption layer, extra gas molecule equably disperse around Nano diamond.Then pass to inertia protection gas
Body enables adsorbate pyrolytic deposition in situ under the conditions of certain temperature.Since above-mentioned absorption-pyrolytic reaction is by adsorption
The gas gross control that layer is passed through from limited reactions, thus silicon cladding can be promoted along surface two-dimensional growth, form quasiatom
Grade coating.
Since silane belongs to flammability hazard gas, silane pyrolysis deposition quasiatom silicon plating is realized on Nano diamond surface
Layer, equipment sedimentary condition and safe handling condition are more harsh, and general chemical vapor depsotition equipment cannot achieve.Therefore, it needs
Develop a kind of dedicated Nano diamond silane surface vacuum pyrolysis depositing device.
Summary of the invention
The present invention provides a kind of Nano diamond surface cleaning, realize that the vacuum pyrolysis deposition of quasiatom grade silicon cladding is set
It is standby.Specifically, the equipment includes vacuum tube furnace, quartz ampoule, objective table, flowmeter, compound vacuum gauge, the equipment is also set
It is equipped with: mechanical pump, diffusion pump, four-way valve, silane air inlet, argon inlet mouth, vent valve, ring groove flange;
The quartz ampoule is arranged in vacuum tube furnace, the four-way of described quartz ampoule one end high-vacuum tube and four-way valve
It is connected, the of four-way valve is equipped with reactive valve between four-way and quartz ampoule, the other end of quartz ampoule is provided with ring groove flange, annular groove
The face flange other side is connect with the external world with vent valve, and the objective table that can hold Nano diamond is provided in the quartz ampoule,
The quartz ampoule having a size ofThe reaction chamber that it is deposited as silane pyrolysis;
The compound vacuum gauge leads to the first of the four-way valve and is connected, and the other end is connected with diffusion pump;It is described compound true
Vacuum pumping valve is equipped between the first of sky meter and four-way valve is logical;The of four-way valve is equipped with reactive valve between four-way and quartz ampoule;
One end of the flowmeter leads to the second of the four-way valve and is connected, and the other end is connected with silane air inlet;It is described
Four-way valve second it is logical connected between the silane air inlet with high-vacuum tube, flow is controlled using silane valve;
The mechanical pump is connect with the diffusion pump with low vacuum tube;The diffusion pump is through the compound vacuum gauge and institute
The first of the four-way valve stated is logical to be connected;
It is connected between the argon inlet mouth is logical with the third of the four-way valve using the vacuum hose of DN8;Using argon gas
Valve controls flow.
Preferably, the range of the compound vacuum gauge (10) is 0-10-6Pa。
Preferably, the vacuum pumping valve, silane valve, argon gas valve, reactive valve and four-way valve connect, connection type phase
Together, using stainless-steel vacuum clamp connection.
Preferably, being connect between the vent valve (11) and ring groove flange (12) using welding manner.
Nano diamond silane surface vacuum pyrolysis depositing device provided by the present invention, has the advantages that
(1) by the cooperation of each component, so that silane gas is fully infiltrated into the Nano diamond powder of accumulation under negative pressure
Between, realize absorption-pyrolytic reaction, the gas gross which is passed through by surface absorbed layer controlled from limited reactions, thus
Silicon cladding can be promoted along surface two-dimensional growth, form quasiatom grade coating.
(2) mechanical pump and diffusion pump are connected with low vacuum tube, be may be implemented first to take out low vacuum, be laid the groundwork for high vacuum environment
Effect.
(3) by the cooperation of each valve gas circuit, it can be realized the purified treatment Nano diamond under high vacuum state, make it
A large amount of oxygen-containing, nitrogenous, desorptions of functional group containing Cl of adsorption.Silane gas is imported after being cooled to room temperature into reaction chamber,
It is fully infiltrated under negative pressure between the Nano diamond powder of accumulation.
(4) range of compound vacuum gauge is 0-10-6Pa, can measure the vacuum degree in high vacuum system, and ultimate vacuum≤
1x10-6Pa。
(5) high-vacuum tube is connected with quartz test tube with annular groove face flanged joint;Quartz test tube and vent valve sealing suit
Structure connection, may be implemented the sealing by a few road sealing rings, and the available effective guarantee of leakproofness guarantees required when deposition
High vacuum environment, security hidden trouble when effectively silane gas being avoided to use.Movable dog structure is devised, object is unloaded and is set
Clip need to be only unscrewed when object, removes end cap, quartzy objective table can be taken out or built-in.Both facilitated in this way sample placement and
It takes out, also spreads out with ensure that nano-diamond powder energy even uniform simultaneously.
(6) vacuum pumping valve, silane valve, argon gas valve, reactive valve and four-way valve connect, and connection type is identical, using not
The steel vacuum clamp that becomes rusty connects, it is ensured that required high vacuum environment when deposition.Pass through the cooperation on valve road, part precursor molecule
It reacts to form unimolecule or polymolecular saturation adsorption layer, the equably disperse of extra gas molecule with Nano diamond surface dangling bond
Around Nano diamond.It then passes to inert protective gas and is pyrolyzed adsorbate in situ and receiving
Rice diamond surface forms silicon cladding.The uniform plating of quasiatom silane coating layer, and thickness is about 0.5nm~10nm.
(7) vent valve and annular groove face flanged joint, are connected, it is ensured that required Gao Zhen when deposition with welding manner
Altitude, security hidden trouble when effectively silane gas being avoided to use.
(8) quartz test tube described in having a size ofThe reaction chamber that it is deposited as silane pyrolysis, it is ensured that receive
Rice diamond uniform is heated, and depositing temperature is about 300 DEG C~650 DEG C continuously adjustable, and warm area stability is ± 1 DEG C.
Detailed description of the invention
Fig. 1 is the assembling schematic diagram of Nano diamond silane surface vacuum pyrolysis depositing device;
Fig. 2 is end seals sleeve structure schematic diagram;
Fig. 3 is silicon atom plating Nano diamond transmission electron microscope picture;
Specific embodiment
In conjunction with attached drawing 1,2 as it can be seen that a kind of Nano diamond silane surface vacuum pyrolysis depositing device, including 1 He of mechanical pump
Vacuum pump 2, by four-way valve 3 by silane air inlet 7, protective gas argon inlet mouth 8 and 5 phase of quartz ampoule in vacuum tube furnace 4
Even, required high vacuum environment when guaranteeing silane plating.Nano diamond is placed on the objective table 6 of 5 the inside of quartz ampoule,
Purified treatment Nano diamond in high vacuum, hot environment makes a large amount of oxygen-containing, nitrogenous, solutions of functional group containing Cl of its adsorption
It inhales.Silane gas is imported after being cooled to room temperature into reaction chamber, flowmeter 9 controls the content for being passed through silane, is allowed to fill under negative pressure
Divide between the Nano diamond powder for penetrating into accumulation.Part silane gas reacts to form unimolecule with Nano diamond surface dangling bond
Or polymolecular be saturated adsorption layer, and equably disperse around Nano diamond.Then protective gas is passed through from argon inlet mouth 8
Argon gas is pyrolyzed adsorbate in situ in Nano diamond surface formation silicon cladding.Wherein, vacuum degree passes through compound vacuum gauge 10
It measures.
Specifically, the Nano diamond silane surface vacuum pyrolysis depositing device, including vacuum tube furnace 4, quartz ampoule
5, objective table 6, flowmeter 9, compound vacuum gauge 10, the equipment are additionally provided with: mechanical pump 1, diffusion pump 2, four-way valve 3, silane
Air inlet 7, argon inlet mouth 8, vent valve 11, ring groove flange 12;
The quartz ampoule 5 is arranged in vacuum tube furnace 4, and the of 5 one end high-vacuum tube of quartz ampoule and four-way valve 3
Four-way is connected, and reactive valve is equipped between the four-way and quartz ampoule 5 of four-way valve 3, and the other end of quartz ampoule 5 is provided with annular groove face method
Orchid 12,12 other side of ring groove flange are connect with the external world with vent valve 11, and nanogold can be held by being provided in the quartz ampoule 5
The objective table 6 of hard rock, the quartz ampoule 5 having a size ofThe reaction chamber that it is deposited as silane pyrolysis;
The compound vacuum gauge 10 leads to the first of the four-way valve 3 and is connected, and the other end is connected with diffusion pump 2;It is described multiple
Close vacuum meter 10 and four-way valve 3 first it is logical between be equipped with vacuum pumping valve;It is equipped between the four-way and quartz ampoule 5 of four-way valve anti-
Answer valve;
One end of the flowmeter 9 leads to the second of the four-way valve 3 and is connected, and the other end is connected with silane air inlet 7;Institute
The second of the four-way valve 3 stated is logical to be connected between the silane air inlet 7 with high-vacuum tube, controls flow using silane valve;
The mechanical pump 1 is connect with the diffusion pump 2 with low vacuum tube;The diffusion pump 2 is through the compound vacuum gauge
10 logical are connected with the first of the four-way valve 3;
It is connected between the argon inlet mouth 8 is logical with the third of the four-way valve 3 using the vacuum hose of DN8;Using argon
Air Valve Control flow.
Preferably, the range of the compound vacuum gauge 10 is 0-10-6Pa。
Preferably, the vacuum pumping valve, silane valve, argon gas valve, reactive valve and four-way valve connect, connection type phase
Together, using stainless-steel vacuum clamp connection.
Preferably, being connected between the vent valve 11 and ring groove flange 12 using welding manner.
When work, system vacuumizes and need to first carry out mechanical pump 1 and vacuumize, and reaches 5Pa to its vacuum degree hereinafter, opening diffusion pump
2 make system reach condition of high vacuum degree, and vacuum degree about reaches 8 × 10-3Pa~1 × 10-4Pa can start to heat system;Heating carries
There are the molybdenum boat and reaction cavity of Nano diamond, temperature rises to 400 DEG C~700 DEG C, makes nanogold under condition of high vacuum degree and high temperature
Hard rock surface functional group dangling bond disconnects, then its temperature is down to room temperature;It is first passed through silane gas, inlet period is 1s~40s, silicon
The flow of alkane gas is controlled by flowmeter 9, and flow is 1sccm~1000sccm, silane gas exposure duration in settling chamber
For 1min~50min, silane is made to be adsorbed on diamond surface;Being passed through the argon gas time is 10~80s, and the gas flow of argon gas is
1ml/min~20ml/min, duration of ventilation are 5s~40s;It is begun to warm up after ventilation, is heated to 400 DEG C~600 DEG C, silane
It is decomposed under high temperature, silicon atom is in conjunction with diamond surface dangling bond.The silicon of the atom level of Nano diamond surface attachment at this time.Finally beat
Open air valve 11 will test remaining silane gas using argon gas and disperse discharge reaction cavity.
Fig. 3 is the Nano diamond transmission electron microscope picture after silane plating.Show that Nano diamond surface silicon atoms are plated in figure
Layer is atomic level, and size is about 5nm, realizes the atom level plating of Nano diamond surface silicon.
Claims (4)
1. a kind of Nano diamond silane surface vacuum pyrolysis depositing device, including vacuum tube furnace (4), quartz ampoule (5), loading
Platform (6), flowmeter (9), compound vacuum gauge (10), it is characterised in that: the equipment is additionally provided with: mechanical pump (1), diffusion pump
(2), four-way valve (3), silane air inlet (7), argon inlet mouth (8), vent valve (11), ring groove flange (12);
Quartz ampoule (5) setting is in vacuum tube furnace (4), quartz ampoule (5) one end high-vacuum tube and four-way valve (3)
Four-way be connected, between the four-way and quartz ampoule (5) of four-way valve (3) be equipped with reactive valve, quartz ampoule (5) the other end setting
Have ring groove flange (12), ring groove flange (12) other side is connect with the external world with vent valve (11), is set in the quartz ampoule (5)
Be equipped with the objective table (6) that can hold Nano diamond, the quartz ampoule (5) having a size ofIt is as silane heat
Solve the reaction chamber of deposition;
The compound vacuum gauge (10) leads to the first of the four-way valve (3) and is connected, and the other end is connected with diffusion pump (2);It is described
Vacuum pumping valve is equipped between the first of compound vacuum gauge (10) and four-way valve (3) is logical;The four-way of four-way valve and quartz ampoule (5) it
Between be equipped with reactive valve;One end of the flowmeter (9) leads to the second of the four-way valve (3) and is connected, the other end and silane air inlet
Mouth (7) is connected;The second of the four-way valve (3) is logical to be connected between the silane air inlet (7) with high-vacuum tube, is used
Silane valve controls flow;
The mechanical pump (1) connect with the diffusion pump (2) with low vacuum tube;The diffusion pump (2) is through described composite evacuated
Meter (10) leads to the first of the four-way valve (3) and is connected;
It is connected between the argon inlet mouth (8) is logical with the third of the four-way valve (3) using the vacuum hose of DN8;Using argon
Air Valve Control flow.
2. Nano diamond silane surface vacuum pyrolysis depositing device according to claim 1, which is characterized in that described
The range of compound vacuum gauge (10) is 0-10-6Pa。
3. Nano diamond silane surface vacuum pyrolysis depositing device according to claim 1, it is characterised in that: described
Vacuum pumping valve, silane valve, argon gas valve, reactive valve and four-way valve connect, and connection type is identical, are connected using stainless-steel vacuum clip
It connects.
4. Nano diamond silane surface vacuum pyrolysis depositing device according to claim 1, which is characterized in that described to put
It is connect between air valve (11) and ring groove flange (12) using welding manner.
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Citations (4)
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CN1235207A (en) * | 1998-04-29 | 1999-11-17 | 微涂技术股份有限公司 | Apparatus and process for controlled atmosphere chemical vapor deposition |
CN104073779A (en) * | 2014-06-20 | 2014-10-01 | 昆明学院 | Organic vapour deposition device and organic vapour deposition method for preparing semiconductor nano material |
CN104561928A (en) * | 2014-12-24 | 2015-04-29 | 浙江大学 | Method for depositing silicon dioxide film on glass substrate |
CN104674186A (en) * | 2015-02-03 | 2015-06-03 | 上海交通大学 | Method for preparing amorphous silicon carbide ceramic-diamond composite coating |
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2016
- 2016-10-17 CN CN201610900669.5A patent/CN106835065B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1235207A (en) * | 1998-04-29 | 1999-11-17 | 微涂技术股份有限公司 | Apparatus and process for controlled atmosphere chemical vapor deposition |
CN104073779A (en) * | 2014-06-20 | 2014-10-01 | 昆明学院 | Organic vapour deposition device and organic vapour deposition method for preparing semiconductor nano material |
CN104561928A (en) * | 2014-12-24 | 2015-04-29 | 浙江大学 | Method for depositing silicon dioxide film on glass substrate |
CN104674186A (en) * | 2015-02-03 | 2015-06-03 | 上海交通大学 | Method for preparing amorphous silicon carbide ceramic-diamond composite coating |
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