CN101921982A - Method for preparing nano-structured nitrogen silicon zirconium coating on surface of hard alloy substrate - Google Patents
Method for preparing nano-structured nitrogen silicon zirconium coating on surface of hard alloy substrate Download PDFInfo
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Abstract
The invention provides a method for preparing a nano-structured nitrogen silicon zirconium coating on the surface of a hard alloy substrate, relating to a hard alloy. A direct-current and radio frequency reaction co-sputtering method is used to prepare the nano-structured nitrogen silicon zirconium coating through controlling the power of a Si target. When the content of Si in a ZrSiN coating is reduced, the Si atoms in the coating exist in the mode of replacing Zr atoms, the ZrSiN coating with low content of Si is solid solution, and the cross section of the ZrSiN coating is in a column structure. The solid solubility and the hardness of the ZrSiN coating are increased with the increment of the content of Si. When the content of Si in the coating reaches a definite amount, excessive element of Si can form amorphous Si3N4 at crystal boundary with element of N. When the content of Si in the coating is further increased, a great amount of amorphous Si3N4 is generated, thus seriously inhabiting the growth of ZrN crystal particles and influencing the degree of crystallization of the coating, in addition, the coating is changed to be in an amorphous state and is in a non-column equiaxial structure.
Description
Technical field
The present invention relates to a kind of Wimet, especially relate to a kind of method for preparing nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces.
Background technology
The research of mechanically resistant material is one of key areas of present Materials science research.Along with developing rapidly of modern manufacturing industry and national defense industry, hard coating material has been widely used in fields such as machinofacture, automotive industry, textile industry, mould industry, space flight and aviation.Coating technology can prepare various functional coatings as the preparation means of material surface technology, and coating is combined with the premium properties of body material, has improved the performance of coated material and body material greatly, has widened range of application.Thereby the material with minute quantity plays a large amount of, expensive integral material role, greatly reduces simultaneously the cost of cutter, reaches the abrasion resistance properties, the processing quality that improves workpiece that improve inserted tool, economizes on resources and the purpose of the energy.In decades, the application of coating technology in cutting tool is the most representative, though because the improvement of cutter material and the exploitation of new cutter material, make cutting speed and machining productivity become the increase of several times even tens times, yet, along with the development of every field technology, the exploitation of modern project material and use increasing ([1] INTERNATIONAL JOURNAL Of REFRACTORYMETALS AND HARD MATERIALS 24 (2006) 399-404).Popularizing rapidly of automatic machine tool, numerically-controlled machine machining center, the development of FMC and system, make mechanical workout towards high-speed, high precision, high-level efficiency and the development of flexibility aspect, cutter many new requirements have been proposed, as the TiN of binary hard coat representative, the needs that the ZrN coating has been difficult to satisfy modern industry, therefore research and develop new cutter coat material, making it have good comprehensive mechanical performance is an extremely important task.
At binary system doping new element, to form the multicomponent composite coating material, make coating have characteristics such as higher hardness, resistance of oxidation, thermohardening, erosion resistance, wearability, this is in the normally used method of new coating material design process.The doping of new element can also reduce the coating internal stress, improves coating toughness, stops crack propagation, improve coating physics and chemical stability.Can add the 3rd group member according to different needs gives the binary coating new characteristic.Summing up various element dopings according to TiN series coating act as in coating: Si, Cr and Y improve resistance of oxidation, Zr, V, C, Hf, Si improve rub resistance wearing and tearing ability, Nb, Ni, W, Zr and Si improve hardness, B, Hf improve the coating bonding force, Hf, Si improve thermostability, and Al improves the coating high-temp performance.As seen the Si element mix the multiple performance that can improve coating, therefore develop tool premium properties ZrSiN coating, and replacement tradition binary coating that will be progressively, become one of focus of present hard coat research field.
The preparation method who mentions about the ZrSiN coating in the existing document roughly divides two kinds: 1. chemical Vapor deposition process ([2] JOURNAL VACUUM SCIENCE TECHNOLOGY 20 (2002) 823-828), the Si element is introduced by tetramethylsilane.2. magnetron sputtering method ([3] SURFACE AND COATINGS TECHNOLOGY 180-181 (2004) 352-256), the zirconium target that embeds silicon chip by argon ion bombardment in nitrogen atmosphere mixes the Si element and forms the ZrSiN coating in the ZrN coating.The particle that chemical Vapor deposition process prepares coating is bigger, and performance is also not as good as the coating of physical vaporous deposition such as magnetron sputtering preparation, and environment is also had certain influence.With respect to chemical vapour deposition, the magnetic sputtering coating particle is the atomic state particle that adopts the cathode sputtering mode to obtain, carry the energy that obtains from target surface and arrive workpiece, form tiny core, rete is organized fine and closely woven [4] SURFACE AND COATINGS TECHNOLOGY 174-175 (2003) 240-245; [5] SCRIPTAMATERIALIA 51 (2004) 715-719), coating performance is good.But the alloys target cost is higher, and is difficult for the Si constituent content in the accurate control coating, and therefore need developing more, reasonable method prepares high-performance ZrSiN coating.
Summary of the invention
The object of the present invention is to provide a kind of employing direct current and radio frequency reaction cosputtering method, prepare the method for nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces.
The present invention includes following steps:
1) substrate pretreated;
2) pre-sputter;
3) sputtering sedimentation.
In step 1), described substrate pretreated can be carried out grinding and polishing, ultrasonic cleaning and ion source successively and be cleaned.
Described grinding and polishing, hard alloy substrate can be roughly ground 10min earlier on 600 purpose boart boart wheel discs, carry out fine grinding 10min then on 1200 purpose boart boart wheel discs, the diamond polishing powder with W2.5 is polished to evenly light of specimen surface again.
Described ultrasonic cleaning can be cleaned the matrix behind the grinding and polishing in the following order, earlier with acetone ultrasonic cleaning 5min, use dehydrated alcohol ultrasonic cleaning 5min then after, dry stand-by.
Described ion source cleans, and can adopt hall ion source that matrix is cleaned 5min, to remove the adsorbed gas and the impurity of matrix surface, improves deposited coatings and high base strength and quality of forming film.
In step 2) in, the condition of described pre-sputter is, substrate temperature is 300 ℃, feed argon gas, regulate the interior operating pressure of sputter cavity to 1Pa, the direct supply power of Zr target is 200W, the radio-frequency power supply power of silicon target material is 100W, pre-sputtering time is 10min, with the nitride of removing target material surface, oxide compound etc., improves the sputter rate of target; Described argon gas and nitrogen gas purity can be 99.99%, and the purity of Zr target can be 99.995%, and the purity of silicon target can be 99.9999%.
In step 3), the condition of described sputtering sedimentation is, after pre-sputter finishes, feed argon gas and nitrogen, total flux is 60sccm, and wherein nitrogen flow is 15%～20%, and sedimentary operating pressure is 0.3～0.5Pa, the direct supply power of Zr target is 250W, the radio-frequency power supply power of silicon target material is 40～80W, and two target surfaces are 90 °, common aura regional alignment hard alloy substrate, sputtering time is 90min, and substrate temperature is 300 ℃; Described argon gas and nitrogen gas purity can be 99.99%, and the purity of Zr target can be 99.995%, and the purity of silicon target can be 99.9999%.
The present invention adopts direct current and radio frequency reaction cosputtering method, prepares the nano-structured nitrogen silicon zirconium hard coat by control Si target power output under conditions such as certain deposition pressure, temperature, nitrogen partial pressure.The chemical ingredients of coating, structure and hardness change with the variation of deposition process conditions.When Si content in the ZrSiN coating reduced, the Si atom existed with the form that replaces the Zr atom in coating, and the ZrSiN coating of therefore low Si content is a sosoloid, and the cross section is a columnar structure.Along with the solid solubility of the increase ZrSiN coating of Si content increases, make hardness increase thereupon.After Si content in the coating reached necessarily, too much the Si element can form non-crystalline state Si with the N element at the crystal boundary place
3N
4Along with the further increase of Si content in the coating can produce a large amount of non-crystalline state Si
3N
4, the growth of severe inhibition ZrN crystal grain influences the degree of crystallinity of coating, so coating becomes non-crystalline state, is axle construction such as non-column.In addition, for the plastic deformation of nano-scale coating is that rotation and atom by crystal grain causes in the migration of crystal boundary, therefore the grain-size along with the increase coating of Si content in the ZrSiN coating reduces, and makes the rotation of crystal grain and the atomic migration of crystal boundary place all become easily, causes hardness decline.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1.In Fig. 1, X-coordinate be diffraction angle 2 θ/°, ordinate zou is diffracted intensity Intensity; 1.26at.%Si represents that the atom percentage content of silicon is 1.26%.
Fig. 2 be embodiment 1 section S EM figure (SEM, * 20,000K).In Fig. 2, scale is 1 μ m.
Fig. 3 is the XRD figure spectrum of embodiment 2.In Fig. 3, X-coordinate be diffraction angle 2 θ/°, ordinate zou is diffracted intensity Intensity; 3.14at.%Si represents that the atom percentage content of silicon is 3.14%.
Fig. 4 is the XRD figure spectrum of embodiment 3.In Fig. 4, X-coordinate be diffraction angle 2 θ/°, ordinate zou is diffracted intensity Intensity; 5.12at.%Si represents that the atom percentage content of silicon is 5.12%.
Fig. 5 is the XRD figure spectrum of embodiment 4.In Fig. 5, X-coordinate be diffraction angle 2 θ/°, ordinate zou is diffracted intensity Intensity; 7.68at.%Si represents that the atom percentage content of silicon is 7.68%%.
Fig. 6 be embodiment 4 section S EM figure (SEM, * 20,000K).In Fig. 6, scale is 1 μ m.
Embodiment
Embodiment 1
1. substrate pretreated: (1) grinding and polishing: hard alloy substrate is roughly ground and fine grinding on 600 orders and 1200 purpose boart boart wheel discs respectively fully, the time of thickness mill is controlled at about 10min, rotating speed is 500r/min, slightly, all to carry out sufficient ultrasonic cleaning (the ultrasonic cleaning time is 2min) and with oven for drying, to remove abrasive dust and greasy dirt between the fine grainding to sample; Sample is through after grinding, and the diamond polishing powder with W2.5 polishes again, and polishing time is 10min.(2) ultrasonic cleaning: the matrix after will polishing cleans in the following order, and acetone ultrasonic cleaning 5min → dehydrated alcohol ultrasonic cleaning 5min → oven dry is stand-by.(3) ion source cleans: before the sputtering sedimentation, adopt hall ion source that matrix is cleaned earlier, the pressure that ion cleans is 2 * 10
-2Pa, 300 ℃ of substrate temperatures, argon gas flux 10sccm, bias voltage is negative 100V, cathodic current voltage is respectively 29.5A, 19V, and anodic current voltage is respectively 7A, 80V, and scavenging period is 5min, to remove the adsorbed gas and the impurity of matrix surface, improve deposited coatings and high base strength and quality of forming film.
2. pre-sputter: during pre-sputter, substrate temperature is 300 ℃, feed argon gas, regulate the interior operating pressure of sputter cavity to 1Pa, the direct supply power of Zr target is 200W, and the radio-frequency power supply power of Si target is 100W, and pre-sputtering time is 10min, with the oxide nitride of removing target material surface etc., improve the sputter rate of target.
3. sputtering sedimentation: pre-sputter finishes the back and feeds argon gas and nitrogen, total flux is 60sccm, wherein nitrogen flow is 15%, sedimentary operating pressure is that the direct supply power of 0.3Pa, Zr target is 250W, the radio-frequency power supply power of Si target is 50W, sputtering time is 90min, and substrate temperature is 300 ℃.After deposition is finished, take out sample and in moisture eliminator, preserve, treat phenetic analysis.
Fig. 1 is the XRD figure spectrum of coating, and the coating that shows preparation is the coating with face-centred cubic structure, and reins in formula according to thanking, and adopting position of (200) diffraction peak and halfwidth calculating grain size calculating grain-size thereof is 19nm.Fig. 2 is the cross section pattern of coating, for columnar structure and organize fine and closely woven.
4. the chemical ingredients of coating adopts EPMA to characterize, and the composition of coating is Zr, Si and N, and its atomic percent is 49.45,1.26% and 49.29%.XRD and EPMA test result show that coating is a solid solution structure.
5. hardness test: the coating hardness testing method is as follows: adopt the nano-indenter test instrument of CSM company, the hardness of coating is calculated as follows: H
IT=F
m/ A
p(H
IT: the hardness of coating; F
m: ultimate load; A
p: the impression shadow area, can calculate by compression distance); According to the variation of thickness, load is set to 10～30mN, and to guarantee compression distance less than 10% of thickness, each sample test is 5 times under the identical conditions, averages, and the mean value that calculates coating hardness is 19.6GPa.
Embodiment 2
1. substrate pretreated: (1) grinding and polishing: with embodiment 1.(2) ultrasonic cleaning: with embodiment 1.(3) ion source cleans: with embodiment 1.
2. pre-sputter: with embodiment 1.
3. sputtering sedimentation: pre-sputter finishes the back and feeds argon gas and nitrogen, total flux is 60sccm, wherein nitrogen flow is 20%, sedimentary operating pressure is 0.3Pa, the direct supply power of Zr target is 250W, the radio-frequency power supply power of Si target is 60W, and sputtering time is 90min, and substrate temperature is 300 ℃.After deposition is finished, take out sample and in moisture eliminator, preserve, treat phenetic analysis.After deposition is finished, take out sample and in moisture eliminator, preserve, treat phenetic analysis.
Fig. 3 is the XRD figure spectrum of coating, and the coating that shows preparation is to have face-centred cubic structure.Coated grains size measuring method calculates coated grains and is of a size of 21nm with embodiment 1.
4. the chemical ingredients of coating adopts EPMA to characterize, and the composition of coating is Zr, Si and N, and its atomic percent is 47.38%, 3.14% and 49.48%.XRD and EPMA test result show that coating is a solid solution structure.
5. hardness test: testing method is with embodiment 1, and the mean value that calculates coating hardness is 21.8GPa.
Embodiment 3
1. substrate pretreated: (1) grinding and polishing: with embodiment 1.(2) ultrasonic cleaning: with embodiment 1.(3) ion source cleans: with embodiment 1.
2. pre-sputter: with embodiment 1.
3. sputtering sedimentation: pre-sputter finishes the back and feeds argon gas and nitrogen, total flux is 60sccm, wherein nitrogen flow is 15%, sedimentary operating pressure is 0.5Pa, the direct supply power of Zr target is 250W, the radio-frequency power supply power of Si target is 70W, and sputtering time is 90min, and substrate temperature is 300 ℃.After deposition is finished, take out sample and in moisture eliminator, preserve, treat phenetic analysis.After deposition is finished, take out sample and in moisture eliminator, preserve, treat phenetic analysis.
Fig. 4 is the XRD figure spectrum of coating, and the coating that shows preparation is the coating with face-centred cubic structure.Coated grains size measuring method calculates coated grains and is of a size of 12nm with embodiment 1.
4. the chemical ingredients of coating adopts EPMA to characterize, and the composition of coating is Zr, Si and N, and its atomic percent is 46.23,5.12% and 48.65%.XRD and EPMA test result show that coating is non-crystalline state Si
3N
4Composite structure as crystal boundary parcel nanometer ZrN crystal grain.
5. hardness test: testing method is with embodiment 1, and the mean value that calculates coating hardness is 192GPa.
Embodiment 4
1. substrate pretreated: (1) grinding and polishing: with embodiment 1.(2) ultrasonic cleaning: with embodiment 1.(3) ion source cleans: with embodiment 1.
2. pre-sputter: with embodiment 1.
3. sputtering sedimentation: pre-sputter finishes the back and feeds argon gas and nitrogen, total flux is 60sccm, wherein nitrogen flow is 20%, sedimentary operating pressure is 0.5Pa, the direct supply power of Zr target is 250W, the radio-frequency power supply power of Si target is 80W, and sputtering time is 90min, and substrate temperature is 300 ℃.After deposition is finished, take out sample and in moisture eliminator, preserve, treat phenetic analysis.After deposition is finished, take out sample and in moisture eliminator, preserve, treat phenetic analysis.
Fig. 5 is the XRD figure spectrum of coating, shows that the degree of crystallinity of coating of preparation is very low.Can't rein in the grain size that formula calculates coating according to thanking.
Fig. 6 is the section S EM pattern of coating, compares with embodiment 1, and the cross section becomes axle construction such as non-column.
4. the chemical ingredients of coating adopts EPMA to characterize, and the composition of coating is Zr, Si and N, and its atomic percent is 44.09%, 7.68% and 48.23%.XRD and EPMA test result show that coating is an amorphous structure.
5. hardness test: testing method is with embodiment 1, and the mean value that calculates coating hardness is 16.7GPa.
Claims (9)
1. prepare the method for nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces, it is characterized in that may further comprise the steps:
1) substrate pretreated;
2) pre-sputter;
3) sputtering sedimentation.
2. as claimed in claim 1ly prepare the method for nano-structured nitrogen silicon zirconium coating, it is characterized in that in step 1) described substrate pretreated is to carry out grinding and polishing, ultrasonic cleaning and ion source successively to clean in cemented carbide substrate surfaces.
3. the method for preparing nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces as claimed in claim 2, it is characterized in that in step 1), described grinding and polishing, be that hard alloy substrate is roughly ground 10min earlier on 600 purpose boart boart wheel discs, carry out fine grinding 10min then on 1200 purpose boart boart wheel discs, the diamond polishing powder with W2.5 is polished to evenly light of specimen surface again.
4. the method for preparing nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces as claimed in claim 2, it is characterized in that in step 1), described ultrasonic cleaning, be that the matrix behind the grinding and polishing is cleaned in the following order, earlier with acetone ultrasonic cleaning 5min, after using dehydrated alcohol ultrasonic cleaning 5min then, dry stand-by.
5. as claimed in claim 2ly preparing the method for nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces, it is characterized in that in step 1) described ion source cleans, is to adopt hall ion source that matrix is cleaned 5min.
6. the method for preparing nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces as claimed in claim 1, it is characterized in that in step 2) in, the condition of described pre-sputter is, substrate temperature is 300 ℃, feed argon gas, regulate the interior operating pressure of sputter cavity to 1Pa, the direct supply power of Zr target is 200W, the radio-frequency power supply power of silicon target material is 100W, and pre-sputtering time is 10min.
7. the method for preparing nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces as claimed in claim 1, it is characterized in that in step 2) in, described argon gas and nitrogen gas purity are 99.99%, and the purity of Zr target is 99.995%, and the purity of silicon target is 99.9999%.
8. the method for preparing nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces as claimed in claim 1, it is characterized in that in step 3), the condition of described sputtering sedimentation is, after pre-sputter finishes, feed argon gas and nitrogen, total flux is 60sccm, wherein nitrogen flow is 15%～20%, sedimentary operating pressure is 0.3～0.5Pa, and the direct supply power of Zr target is 250W, and the radio-frequency power supply power of silicon target material is 40～80W, two target surfaces are 90 °, common aura regional alignment hard alloy substrate, sputtering time is 90min, substrate temperature is 300 ℃.
9. the method for preparing nano-structured nitrogen silicon zirconium coating in cemented carbide substrate surfaces as claimed in claim 1, it is characterized in that in step 3), described argon gas and nitrogen gas purity are 99.99%, and the purity of Zr target is 99.995%, and the purity of silicon target is 99.9999%.
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