CN105274485A - Preparation method for Cr-Si-C-N nano composite film - Google Patents
Preparation method for Cr-Si-C-N nano composite film Download PDFInfo
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- CN105274485A CN105274485A CN201510783525.1A CN201510783525A CN105274485A CN 105274485 A CN105274485 A CN 105274485A CN 201510783525 A CN201510783525 A CN 201510783525A CN 105274485 A CN105274485 A CN 105274485A
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Abstract
The invention discloses a preparation method for a Cr-Si-C-N nano composite film. The preparation method comprises the following steps that (1) ultrasonic cleaning is conducted for 30 min through a KH-100B ultrasonic cleaning instrument, and base materials (316L stainless steel discs, titanium alloy discs and monocrystalline silicon pieces) which are cleaned and dried are clamped on a working stage; (2) the base materials are bombarded through Ar<+> ion beams for 30 min, and the base materials are cleaned and activated; (3) argon is introduced, a direct-current Cr target is started, and a transition Cr layer is deposited; and (4) mixed gas of high-purity argon and nitrogen is introduced, the direct-current Cr target and a radio frequency C target are started, different flows of trimethylsilane (TMS) are set, sputtering is conducted through a UDP-650 unbalanced magnetron sputtering system, and the Cr-Si-C-N nano composite film is deposited on the base materials. According to the Cr-Si-C-N nano composite film prepared through the preparation method, grains are refined through doping of Si, the internal stress of the film is lowered, and the hardness of the nano composite film is improved, so that the friction coefficient and the abrasion amount of the film are reduced, the corrosion resistance and oxidization resistance of the film are improved, and the Cr-Si-C-N nano composite film is better in mechanical property.
Description
Technical field:
The present invention relates to tribology and Surface Engineering field, specifically, that relate to is a kind of preparation method of Cr-Si-C-N nano compound film.
Background technology:
Based on the fundamental research problem of resources conservation and environmentally friendly water lubricating surface of friction pair film, become the focus that developed country is competitively studied.In order to make Cr-C-N base film obtain excellent water lubricating tribological property, Composition Design and modification are carried out to Cr-C-N base film.And for magnesium-yttrium-transition metal carbonitride, the formation of its interface friction layer is main relevant with the friction hydration reaction of friction pair.If friction pair material is easy to the hydration reaction that rubs, generate frictional interface layer, then its frictional coefficient reduces.In order to make Cr-C-N base film obtain excellent water lubricating tribological property, Composition Design and modification must be carried out based on hydration reaction theory to Cr-C-N base film.Research shows, silicide shows the Si (OH) that excellent water lubricating performance is all formed with frictional interface hydration reaction in water
4lubricant film is relevant.If add Si in Cr-C-N film, then Cr-Si-C-N coating formation with Cr (C, N) for crystalline phase, Si
3n
4be the nanocrystalline composite coating of amorphous phase with SiC.By changing the flow of silane, thus change the content of Si in coating, hardness presents the Changing Pattern of first increases and then decreases.Its grain-size, phase structure and formation Si
3n
4with factors such as the content of SiC amorphous phase, abrasion resistance tool in the mechanics of film and water lubricating thereof is had a certain impact.
Summary of the invention:
The object of this invention is to provide a kind of preparation method of Cr-Si-C-N nano compound film, by changing the flow of silane (TMS), obtain the nano compound film with different Si content, make it that there is low internal stress, strong film-substrate cohesion, the Cr-Si-C-N nano compound film of good thermal stability and abrasion resistance.
The present invention adopts following technical scheme: a kind of preparation method of Cr-Si-C-N nano compound film, it comprises the steps:
(1) open UDP-650 type unbalanced magnetron sputtering system vacuum chamber door, by clean the base material clamping that dries up on Stage microscope after, close this sputtering system vacuum chamber door;
Etc. (2) background vacuum is evacuated to the 10-4Pa order of magnitude, holding chamber temperature 200 DEG C in vacuum, and the residual water-content in cavity is evaporated sooner;
Etc. (3) after cavity temperature drops to room temperature, pass into Ar gas, open d.c. sputtering target, ion beam cleaning 30min is carried out to base material, remove substrate surface pollutent and activated substrate is surperficial;
(4) keep Stage microscope speed of rotation 10rpm, pass into high-purity argon gas, the stable gas pressure in cavity is 4.0 ~ 5.0 × 10
-1pa, regulates the sputtering current 4.0A of Metal Cr target, keeps base material negative bias-80V, dutycycle 50%, base material temperature Rt=300 DEG C, at room temperature deposits 9 minutes, deposition transition Cr layer;
(5) pass into the mixed gas of high-purity argon gas and nitrogen, pass into trimethyl silane or the tetramethylsilane of different flow, the stable gas pressure in cavity is 4.0 ~ 5.0 × 10
-1pa, changes the flow of silane, regulates magnetically controlled DC sputtering Metal Cr target current to be 4.0A, and regulate magnetically controlled DC sputtering C target current to be 1.0A, base material negative bias is-80V, and dutycycle is 50%, base material temperature R
t=100 ~ 300 DEG C, depositing time is 80min, and rotatable stage prepares Cr-Si-C-N nano compound film on base material.
Further, base material is monocrystalline silicon piece or stainless steel or titanium alloy in step (1).
Further, in step (1) by the single crystalline Si sheet of well cutting and stainless steel, titanium alloy at acetone, carry out ultrasonic cleaning in alcohol and deionized water, stand-by after dry.
Further, d.c. sputtering target is opened in step (3), wherein the distance of base material and target remains on 7 ~ 8cm, Ar airshed 20 ~ 40sccm, ionic fluid bias voltage-450V, dutycycle 50%, carries out ion beam cleaning 30min to base material, removes substrate surface pollutent activated substrate is surperficial.
The present invention has following beneficial effect:
(1) can at room temperature deposit film, greatly reduce the restriction that base material is selected;
(2) in Cr-Si-C-N, the content of Metal Cr, nonmetal C can be regulated by magnetically controlled DC sputtering target current, and the content of Si regulates by controlling silane flow rate;
(3) preparation technology is simple, and operation motility is good.
Accompanying drawing illustrates:
Fig. 1 is unbalanced magnetron sputtering system schematic diagram.
Fig. 2 is each constituent content in the Cr-Si-C-N film prepared under different silane flow rate.
Fig. 3 is hardness and the Young's modulus of the Cr-Si-C-N film prepared under different silane flow rate.
Fig. 4 is the X-ray diffraction spectrum of the Cr-Si-C-N nano compound film prepared under different silane flow rate.
Fig. 5 is the scanning electron microscope (SEM) photograph of the Cr-Si-C-N nano compound film prepared under different silane flow rate.
Embodiment:
Please refer to shown in Fig. 1, the present invention adopts the method for non-balance magnetically controlled sputter to prepare, and the method can at a lower temperature, at nearly all deposited on substrates Cr-Si-C-N nano compound film.
Specifically comprise the following steps:
(1) open UDP-650 type unbalanced magnetron sputtering system vacuum chamber door, base material clamping cleaning dried up is on Stage microscope, and wherein base material is monocrystalline silicon piece or stainless steel, closes this sputtering system vacuum chamber door;
(2) the chamber vacuum degree of unbalanced magnetron sputtering system is evacuated to the 10-4Pa order of magnitude, holding chamber temperature 200 DEG C in vacuum, makes the residual water-content in cavity evaporate sooner;
Etc. (3) after cavity temperature drops to room temperature, pass into Ar gas, open d.c. sputtering target, wherein the distance of base material and target remains on 7 ~ 8cm, Ar airshed 20 ~ 40sccm, ionic fluid bias voltage-450V, dutycycle 50%,
Ion beam cleaning 30min is carried out to base material, removes substrate surface pollutent activated substrate is surperficial;
(4) Stage microscope speed of rotation 10rpm is kept, pass into high-purity argon gas, stable gas pressure in cavity is at 4.0 ~ 5.0 × 10-1Pa, regulate the sputtering current 4.0A of Metal Cr target, keep base material negative bias-80V, dutycycle 50%, base material temperature Rt=300 DEG C, at room temperature deposit 9 minutes, deposition transition Cr layer.
(5) pass into the mixed gas of high-purity argon gas and nitrogen, pass into trimethylammonium (tetramethyl-) silane of different flow, the stable gas pressure in cavity is 4.0 ~ 5.0 × 10
-1pa, changes the flow of silane, regulates magnetically controlled DC sputtering Metal Cr target current to be 4.0A, and regulate magnetically controlled DC sputtering C target current to be 1.0A, base material negative bias is-80V; Dutycycle is 50%; Base material temperature R
t=100 ~ 300 DEG C; Depositing time is 80min, and rotatable stage prepares Cr-Si-C-N nano compound film on base material.
The preparation method of Cr-Si-C-N nano compound film of the present invention is described below by specific embodiment.
Embodiments of the invention are specifically implemented according to following steps:
(1) base material prepares
With natural diamond glass cutter, single crystalline Si sheet is cut into 5 × 5cm2 fritter, 316L stainless steel cut becomes
the disk of thick 6mm, is polished to roughness Ra=50nm.By the single crystalline Si sheet of well cutting and stainless steel at acetone, in alcohol and deionized water, carry out ultrasonic cleaning, stand-by after dry.
(2) target and base material Ion Cleaning
When being evacuated to the 10-4Pa order of magnitude Deng background vacuum, pass into Ar gas (20 ~ 40sccm), radio frequency negative bias-450V, dutycycle 50%, utilize Ar+ ion bombardment substrate surface, remove pollutent and the activated deposition surface of substrate surface, scavenging period 30min.
(3) deposit film transition Cr layer
Keep Stage microscope speed of rotation 10rpm, pass into high-purity argon gas, wait stable gas pressure in cavity after 4.0 ~ 5.0 × 10-1Pa, regulate the sputtering current 4.0A of Metal Cr target, keep bias voltage-80V, dutycycle 50%, at room temperature deposit 9 minutes, deposition transition Cr layer.
(4) film preparation
Pass into the mixed gas of high-purity argon gas and nitrogen (because the dividing potential drop of nitrogen reactive gas monitors (OEM) control by the optical emitting of rapid feedback, this feedback procedure is the spectral line of emission by observing splash-proofing sputtering metal target, therefore, a quick response dynamics is utilized to adjust piezo electric valve to control the flow of nitrogen.In the present invention, pass into the mixed gas of argon gas and nitrogen, the OEM generating nitride is set to 50%), change the flow passing into silane, the stable gas pressure in cavity is 4.0 ~ 5.0 × 10
-1sputtering current on Pa, adjustment Cr target is the sputtering current on 4.0A and C target is 1.0A, regulates base material negative bias-80V, dutycycle 50%, base material temperature R
t=100 ~ 300 DEG C; Depositing time is 80min, and rotatable stage prepares Cr-Si-C-N nano compound film on base material.
Embodiment 1
(1) base material and target prepare
With 5 × 5cm
2single crystalline Si (100) sheet and
316L medical stainless steel as base material, 316L stainless steel is polished and is polished to roughness Ra=50nm, then by single crystalline Si (100) sheet and 316L stainless steel successively at acetone, carry out ultrasonic cleaning in alcohol and deionized water, last electricity consumption dries up.Metal Cr and C target are arranged on respective magnetically controlled DC sputtering target holder respectively.
(2) target and base material Ion Cleaning
The 10-4Pa order of magnitude is reached Deng background vacuum, open and turn Stage microscope, pass into Ar gas, setting base material negative bias-80V, dutycycle 50%, utilize Ar+ ion bombardment single crystalline Si (100) sheet and 316L stainless steel surface, remove pollutent and the activated deposition surface of substrate surface further, cleaning base material 30 minutes.
(3) film transition Cr layer deposition
Keep Stage microscope speed of rotation 10rpm, pass into high-purity argon gas, wait stable gas pressure in cavity 4.0 ~ 5.0 × 10
-1after Pa, regulate the sputtering current 4.0A of Metal Cr target, keep bias voltage-80V, dutycycle 50%, under room temperature (Rt), deposit 9 minutes, deposition transition Cr layer.
(4) film preparation
Keep Stage microscope speed of rotation 10rpm, pass into the mixed gas (OEM50%) of high-purity argon gas and nitrogen, the stable gas pressure in cavity is 4.0 ~ 5.0 × 10
-1pa, the sputtering current of control Metal Cr target is 4.0A and C target sputtering current is 1.0A, keeps bias voltage-80V, dutycycle 50%, under room temperature (Rt), deposits 80 minutes, preparation Cr-C-N nano-composite coating.
(5) detection of film
1, the detection of each constituent content of film: the content (as Fig. 2) being detected each element of Cr-Si-C-N nano compound film by EDS.
2, the mensuration of hardness: the nano hardness (as Fig. 3) being measured Cr-Si-C-N nano compound film by nano-hardness tester.
3, brilliant molybdenum determination: by the crystal phase structure (as Fig. 4) of X-ray diffraction spectrometry Cr-Si-C-N nano compound film.
4, Cr-Si-C-N nano compound film exterior appearance (as Fig. 5) is measured by scanning electron microscope (SEM).
Embodiment 2
(1) base material and target prepare
With 5 × 5cm
2single crystalline Si (100) sheet and
316L medical stainless steel as base material, 316L stainless steel polishing to roughness Ra=50nm, then by single crystalline Si (100) sheet and 316L medical stainless steel successively at acetone, carry out ultrasonic cleaning in alcohol and deionized water, last electricity consumption dries up.Metal Cr and C target are arranged on respective magnetically controlled DC sputtering target holder respectively.
(2) target and base material Ion Cleaning
10 are reached Deng background vacuum
-4the Pa order of magnitude, open and turn Stage microscope speed of rotation 10rpm, pass into Ar gas, setting base material negative bias-80V, dutycycle 50%, utilize Ar+ ion bombardment single crystalline Si (100) sheet and 316L medical stainless steel surface, remove pollutent and the activated deposition surface of substrate surface, cleaning base material 30 minutes.
(3) film transition Cr layer deposition
Keep Stage microscope speed of rotation 10rpm, pass into high-purity argon gas, wait stable gas pressure in cavity 4.0 ~ 5.0 × 10
-1after Pa, the sputtering current regulating Metal Cr target is 4.0A, and keep bias voltage to be-80V, dutycycle is 50%, under room temperature (Rt), deposit 9 minutes, deposition transition Cr layer.
(4) film preparation
Keep Stage microscope speed of rotation 10rpm, pass into the mixed gas (OEM50%) of high-purity argon gas and nitrogen, pass into silane (TMS) flow 5sccm, stable gas pressure in cavity, at 4.0 ~ 5.0 × 10-1Pa, controls the sputtering current 4.0A of Metal Cr target, C target current 1.0A, keep bias voltage-80V, dutycycle 50%, deposits 80 minutes at 150 DEG C, deposition Cr-Si-C-N nano-composite coating.
Embodiment 3
Steps all in the present embodiment and parameter are all identical with in embodiment 2, only need change silane (TMS) flow in embodiment 2 into 10sccm.
Embodiment 4
Steps all in the present embodiment and parameter are all identical with in embodiment 2, only need change silane (TMS) flow in embodiment 2 into 15sccm.
Embodiment 5
Steps all in the present embodiment and parameter are all identical with in embodiment 2, only need change silane (TMS) flow in embodiment 2 into 20sccm.
Embodiment 6
Steps all in the present embodiment and parameter are all identical with in embodiment 2, only need change silane (TMS) flow in embodiment 2 into 25sccm.
Embodiment 7
Steps all in the present embodiment and parameter are all identical with in embodiment 2, only need change silane (TMS) flow in embodiment 2 into 30sccm.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, can also make some improvement under the premise without departing from the principles of the invention, and these improvement also should be considered as protection scope of the present invention.
Claims (4)
1. a preparation method for Cr-Si-C-N nano compound film, is characterized in that: comprise the steps
(1) open unbalanced magnetron sputtering system vacuum chamber door, by clean the base material clamping that dries up on Stage microscope after, close this sputtering system vacuum chamber door;
Etc. (2) background vacuum is evacuated to 10
-4the Pa order of magnitude, holding chamber temperature 200 DEG C in vacuum, makes the residual water-content in cavity evaporate sooner;
Etc. (3) after cavity temperature drops to room temperature, pass into Ar gas, open d.c. sputtering target, ion beam cleaning 30min is carried out to base material, remove substrate surface pollutent and activated substrate is surperficial;
(4) keep Stage microscope speed of rotation 10rpm, pass into high-purity argon gas, the stable gas pressure in cavity is 4.0 ~ 5.0 × 10
-1pa, regulates the sputtering current 4.0A of Metal Cr target, keeps base material negative bias-80V, dutycycle 50%, base material temperature Rt=300 DEG C, at room temperature deposits 9 minutes, deposition transition Cr layer;
(5) pass into the mixed gas of high-purity argon gas and nitrogen, pass into trimethyl silane or the tetramethylsilane of different flow, the stable gas pressure in cavity is 4.0 ~ 5.0 × 10
-1pa, changes the flow of silane, regulates magnetically controlled DC sputtering Metal Cr target current to be 4.0A, and regulate magnetically controlled DC sputtering C target current to be 1.0A, base material negative bias is-80V, and dutycycle is 50%, base material temperature R
t=100 ~ 300 DEG C, depositing time is 80min, and rotatable stage prepares Cr-Si-C-N nano compound film on base material.
2. the preparation method of Cr-Si-C-N nano compound film as claimed in claim 1, is characterized in that: in step (1), base material is monocrystalline silicon piece or stainless steel or titanium alloy.
3. the preparation method of Cr-Si-C-N nano compound film as claimed in claim 2, it is characterized in that: in step (1) by the single crystalline Si sheet of well cutting, stainless steel or titanium alloy at acetone, ultrasonic cleaning is carried out in alcohol and deionized water, stand-by after dry.
4. the preparation method of Cr-Si-C-N nano compound film as claimed in claim 1, it is characterized in that: in step (3), open d.c. sputtering target, wherein the distance of base material and target remains on 7 ~ 8cm, Ar airshed 20 ~ 40sccm, ionic fluid bias voltage-450V, dutycycle 50%, carries out ion beam cleaning 30min to base material, removes substrate surface pollutent activated substrate is surperficial.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381471A (en) * | 2016-09-19 | 2017-02-08 | 中国科学院宁波材料技术与工程研究所 | Hardness-width-variable wear-resistant coating, and preparation method and application of wear-resistant coating |
| CN107988577A (en) * | 2017-10-18 | 2018-05-04 | 南京航空航天大学 | A kind of preparation method of CrSiBCN nano compound films |
| CN109778119A (en) * | 2019-01-09 | 2019-05-21 | 南京航空航天大学 | A kind of Ni-CrSiN wear-and corrosion-resistant coating and preparation method thereof |
| CN109957764A (en) * | 2017-12-14 | 2019-07-02 | 中国科学院宁波材料技术与工程研究所 | Water fluid environment CrSiC composite coating and the preparation method and application thereof |
| CN111876735A (en) * | 2020-07-21 | 2020-11-03 | 南京航空航天大学 | Preparation method of wear-resistant and antibacterial Cr-Mo-Ag-Si-C-N multi-element composite film |
| CN113230462A (en) * | 2021-04-08 | 2021-08-10 | 上海微创医疗器械（集团）有限公司 | Medical device |
| CN116043162A (en) * | 2023-03-09 | 2023-05-02 | 中国地质大学（北京） | Nano composite structural coating on surface of titanium alloy cutting tool and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381471A (en) * | 2016-09-19 | 2017-02-08 | 中国科学院宁波材料技术与工程研究所 | Hardness-width-variable wear-resistant coating, and preparation method and application of wear-resistant coating |
| CN107988577A (en) * | 2017-10-18 | 2018-05-04 | 南京航空航天大学 | A kind of preparation method of CrSiBCN nano compound films |
| CN109957764A (en) * | 2017-12-14 | 2019-07-02 | 中国科学院宁波材料技术与工程研究所 | Water fluid environment CrSiC composite coating and the preparation method and application thereof |
| CN109957764B (en) * | 2017-12-14 | 2021-04-02 | 中国科学院宁波材料技术与工程研究所 | CrSiC composite coating for water-based liquid environment and preparation method and application thereof |
| CN109778119A (en) * | 2019-01-09 | 2019-05-21 | 南京航空航天大学 | A kind of Ni-CrSiN wear-and corrosion-resistant coating and preparation method thereof |
| CN111876735A (en) * | 2020-07-21 | 2020-11-03 | 南京航空航天大学 | Preparation method of wear-resistant and antibacterial Cr-Mo-Ag-Si-C-N multi-element composite film |
| CN111876735B (en) * | 2020-07-21 | 2021-11-02 | 南京航空航天大学 | Preparation method of wear-resistant and antibacterial Cr-Mo-Ag-Si-C-N multi-element composite film |
| CN113230462A (en) * | 2021-04-08 | 2021-08-10 | 上海微创医疗器械（集团）有限公司 | Medical device |
| CN116043162A (en) * | 2023-03-09 | 2023-05-02 | 中国地质大学（北京） | Nano composite structural coating on surface of titanium alloy cutting tool and preparation method thereof |
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