CN116814120B - Composite coating applied to dental plate die and preparation method thereof - Google Patents
Composite coating applied to dental plate die and preparation method thereof Download PDFInfo
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- CN116814120B CN116814120B CN202310683536.7A CN202310683536A CN116814120B CN 116814120 B CN116814120 B CN 116814120B CN 202310683536 A CN202310683536 A CN 202310683536A CN 116814120 B CN116814120 B CN 116814120B
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- 238000000576 coating method Methods 0.000 title claims abstract description 118
- 239000011248 coating agent Substances 0.000 title claims abstract description 113
- 239000002131 composite material Substances 0.000 title claims abstract description 107
- 238000002360 preparation method Methods 0.000 title abstract description 75
- 229910001325 element alloy Inorganic materials 0.000 claims abstract description 108
- 239000000843 powder Substances 0.000 claims abstract description 105
- 239000012745 toughening agent Substances 0.000 claims abstract description 101
- 239000002994 raw material Substances 0.000 claims abstract description 75
- 239000011342 resin composition Substances 0.000 claims abstract description 57
- 238000002156 mixing Methods 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 27
- 238000005507 spraying Methods 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 21
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 20
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 19
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 19
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 19
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 18
- 239000004642 Polyimide Substances 0.000 claims abstract description 17
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 17
- 229920001721 polyimide Polymers 0.000 claims abstract description 17
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910000077 silane Inorganic materials 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims description 52
- 238000000498 ball milling Methods 0.000 claims description 48
- 238000005488 sandblasting Methods 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 24
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000003607 modifier Substances 0.000 claims description 11
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000007822 coupling agent Substances 0.000 claims description 4
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical group [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 239000000853 adhesive Substances 0.000 abstract description 5
- 230000001070 adhesive effect Effects 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 36
- 230000000052 comparative effect Effects 0.000 description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- 239000010431 corundum Substances 0.000 description 11
- 229910052593 corundum Inorganic materials 0.000 description 11
- 239000004576 sand Substances 0.000 description 11
- 239000007921 spray Substances 0.000 description 11
- 238000005238 degreasing Methods 0.000 description 10
- 229910052759 nickel Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 229910052702 rhenium Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 229910003849 O-Si Inorganic materials 0.000 description 1
- 229910003872 O—Si Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000641 cold extrusion Methods 0.000 description 1
- WUPRCGRRQUZFAB-DEGKJRJSSA-N corrin Chemical compound N1C2CC\C1=C\C(CC/1)=N\C\1=C/C(CC\1)=N/C/1=C\C1=NC2CC1 WUPRCGRRQUZFAB-DEGKJRJSSA-N 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)
Abstract
The application relates to the technical field of functional coating materials, and particularly discloses a composite coating applied to a dental plate die and a preparation method thereof, wherein the composite coating comprises a resin composition, a toughening agent and multi-element alloy micro powder; the resin composition includes polytetrafluoroethylene and polyimide; the toughening agent is prepared by mixing graphene oxide with liquid sodium silicate and then modifying the mixture by silane; the multi-element alloy micro powder comprises raw materials Mo, ni, V, co, re and Mn; the preparation method of the composite coating comprises the steps of premixing a toughening agent and multi-element alloy micro powder, adding the mixture into a resin composition, uniformly stirring, spraying the mixture onto the surface of a dental plate die to be sprayed, and curing the mixture to obtain the required composite coating; the preparation method is simple, the preparation condition is mild, the preparation method is suitable for industrial production, the obtained composite coating has high wear resistance, good toughness, high bonding strength with a die and good adhesive force, and is suitable for industrial application.
Description
Technical Field
The application relates to the technical field of functional coating materials, in particular to a composite coating applied to a dental plate die and a preparation method thereof.
Background
The die plate die is used for two square templates on the thread rolling machine, is made of DC53 material or SKH-9 high-speed steel, is divided into two blocks, the long plate is a movable tooth plate, the short plate is a fixed tooth plate, and the upper surface of the long plate is provided with tooth grains for extruding and forming the screw mercerized nails into threads. The screw plate die is a screw tool most commonly used in the standard fastener industry for processing screws and bolts, the processing principle mainly adopts cold extrusion molding, a fixed screw plate and a movable screw plate of the screw plate die clamp the screws therebetween, and a driving device of the screw plate die drives the movable screw plate to move parallel to the fixed screw plate, so that screw finished products are formed by matching opposite threads on the acting surfaces of the two screw plates in a twisting extrusion processing mode. The die plate die has bad service conditions, and the interaction between the screw rod and the die leads to very complex stress conditions on the inner surface of the die, so that the die can fail due to deformation, fatigue crack on the inner surface and the like. In the processing process, the surface of the die bears the high-pressure friction action of the screw rod to cause abrasion, deformation is generated to influence the precision of the screw rod, and the service life of the die is greatly shortened due to failure of the die.
In the related art, in order to improve the wear resistance of dental plate molds and extend the service life thereof, one or more composite wear-resistant coatings are generally prepared on the surfaces of the molds, and common surface coating techniques such as surface chromium plating, nickel, physical (chemical) vapor deposition, arc ion plating, and magnetron sputtering hard coatings such as TiN, crN, tiAlN are used. The surface treatment methods are widely applied in industry, but have the problems of poor body toughness, low interface bonding strength between the coating and the surface of the die and the like of the coating such as chromium, nickel, tiN, crN, tiAlN and the like coated on the surface, and restrict the manufacture and the use of the dental plate die. Based on the above statement, the application provides a composite coating applied to a dental plate die and a preparation method thereof, and aims to improve the wear resistance of the dental plate die and the toughness of a coating body and the bonding capability of the coating and the die.
Disclosure of Invention
In order to solve the problems of poor toughness, low bonding strength between a coating and a die and the like of the abrasion-resistant coating body of the current dental plate die, the application provides a composite coating applied to the dental plate die and a preparation method thereof.
In a first aspect, the present application provides a composite coating, which adopts the following technical scheme:
the composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100-120 parts of resin composition, 3-5 parts of toughening agent and 8-12 parts of multi-element alloy micropowder;
the resin composition comprises polytetrafluoroethylene, polyimide and polyvinyl alcohol aqueous solution in a mass ratio of 5-8:1:0.1-0.3;
the toughening agent is prepared by mixing graphene oxide with liquid sodium silicate, and then modifying the mixture by silane;
the multi-element alloy micro powder comprises a raw material Mo, ni, V, co, re and Mn.
Preferably, the composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 110 parts of resin composition, 4 parts of toughening agent and 10 parts of multi-element alloy micropowder.
Preferably, the toughening agent is prepared by the following method:
and controlling the mass ratio of graphene oxide to liquid sodium silicate to silane coupling agent to be 1:0.2-0.3:0.1, mixing the graphene oxide with the liquid sodium silicate, performing first ball milling treatment, adding the silane coupling agent, performing second ball milling treatment, and modifying to obtain the required toughening agent.
Preferably, the ball milling medium is stainless steel ball with the diameter of 10-20 mu m, and the ball-material ratio is 3-4:1.
Preferably, the rotation speed of the first ball milling is 400-600r/min, and the ball milling time is 1-3h; the second ball milling rotating speed is 200-300r/min, and the ball milling time is 1-2h.
Preferably, the silane coupling agent is an aminosilane coupling agent.
Preferably, the multi-element alloy micro powder comprises 8.2-13.5% of Mo, 2.3-4.4% of Ni, 0.5-0.8% of V, 0.2-0.3% of Co, 0.01-0.05% of Re and the balance of Mn in percentage by weight.
Preferably, the multi-element alloy micro powder is prepared by the following method:
(1) Weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinder together, and grinding and mixing uniformly to obtain nano alloy powder;
(2) Adding modifier into the nano mixed powder according to the mass ratio of 1:0.1-0.2, continuously grinding and mixing for 1-3h, and drying to obtain the needed multi-element alloy micro powder.
Preferably, the grinding pressure in the step (1) is 60-80kPa, the grinding rotating speed is 20-50r/min, and the grinding time is 30-70min.
Preferably, the modifier in the step (2) is a compound of methyl ethylene oxide and dodecanol in a mass ratio of 2-3:1.
Preferably, the drying temperature in the step (2) is 380-460 ℃ and the drying time is 3-5h.
In a second aspect, the application provides a method for preparing a composite coating applied to a dental plate die, which adopts the following technical scheme:
the preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning and drying the dental plate die, and then performing sand blasting treatment to obtain the dental plate die to be sprayed;
s3, after premixing the toughening agent and the multi-element alloy micro powder uniformly, adding the toughening agent and the multi-element alloy micro powder into the resin composition, and stirring and mixing uniformly to obtain a composite coating raw material;
and S4, spraying the composite coating raw material on the surface of the die to be sprayed, and carrying out vacuum curing to obtain the required composite coating.
Preferably, in the step S2, white corundum micropowder with the particle size of 60-100 μm is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5-0.8MPa, the distance between the nozzle and a die plate die is 20-30mm, and the sand blasting angle is 50-80 degrees.
Preferably, in the step S3, the stirring and mixing rotating speed is 200-800r/min, and the stirring time is 10-80min.
Preferably, the spraying parameters in the step S4 are as follows: the spraying temperature is 20-40 ℃, the spraying distance is 18-30mm, the moving speed of the spray gun is 20-28mm/s, the overlap joint amount of adjacent passes is 1-2mm, and the thickness of the composite coating is 150-400 mu m.
Preferably, the vacuum curing conditions in the step S4 are as follows: curing for 1-2h in a vacuum environment at 220-280 ℃.
In summary, the application has the following beneficial effects:
according to the resin composition, polytetrafluoroethylene, polyimide and a polyvinyl alcohol aqueous solution are compounded, polyimide with excellent mechanical properties and high temperature resistance is added by controlling the proportion, so that the high temperature wear resistance of the composite coating and the bonding strength of the composite coating and a dental plate die can be enhanced, and meanwhile, the polyvinyl alcohol aqueous solution is added, so that intermolecular interaction force can be formed between the polytetrafluoroethylene and the polyimide, and the compatibility of the polytetrafluoroethylene and the polyimide is improved.
According to the preparation method, after graphene oxide is mixed with liquid sodium silicate for modification, silane is added for modification to obtain a toughening agent, firstly Na+ ions in liquid sodium silicate molecules can interact with negative charges on the surface of graphene oxide, so that the surface property of the graphene oxide is improved, the compatibility, the dispersibility and the stability of the graphene oxide are improved, in addition, si-O-Si bonds in the sodium silicate molecules can form hydrogen bonds with hydroxyl (-OH) on the surface of the graphene oxide, the mechanical property and the stability of the graphene oxide are enhanced, an aminosilane coupling agent is further added for silanization surface functionalization modification, the compatibility and the dispersibility of the graphene oxide are further improved, and further the affinity and the cohesive force of the graphene oxide and a resin composition are improved, and the adhesive force and the toughness of a finally prepared composite coating are improved.
According to the application, mo, ni, V, co, re and Mn are selected as raw materials, methyl ethylene oxide and dodecanol are added for grinding and modifying, and then the mixture is dried to obtain the required multi-element alloy micro powder, and methyl ethylene oxide and dodecanol are utilized for grinding and adsorbing on the surface of the multi-element alloy micro powder to form a layer of compact molecular film, so that the stability, cohesiveness and wear resistance of the multi-element alloy micro powder are enhanced, the bonding strength of the composite coating and a die is further improved, the wear resistance of the composite coating is further improved, and the loss of the composite coating in wear is reduced.
In conclusion, the preparation method disclosed by the application is simple in formula, scientific in proportion, simple in preparation method, mild in preparation condition, high in wear resistance, good in toughness, high in bonding strength with a die, good in adhesive force and suitable for industrial application.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation examples 1-3 and comparative preparation examples 1-2 provide methods for preparing toughening agents.
Preparation example 1
The toughening agent is prepared by the following method:
controlling the mass ratio of graphene oxide (particle size of 30 mu m), liquid sodium silicate (modulus of 3.2) and silane coupling agent KH-792 to be 1:0.2:0.1, mixing the graphene oxide with the liquid sodium silicate, performing first ball milling treatment, adding the silane coupling agent KH-792, performing second ball milling treatment, and modifying to obtain the required toughening agent;
the ball milling medium is a stainless steel ball with the diameter of 10 mu m, the ball-material ratio is 3:1, the ball milling rotating speed of the first time is 400r/min, the ball milling time is 3h, the ball milling rotating speed of the second time is 300r/min, and the ball milling time is 1h.
Preparation example 2
The toughening agent is prepared by the following method:
controlling the mass ratio of graphene oxide (particle size 40 μm), liquid sodium silicate (modulus 3.3) and silane coupling agent KH-540 to be 1:0.25:0.1, mixing the graphene oxide with the liquid sodium silicate, performing a first ball milling treatment, adding the silane coupling agent KH-540, performing a second ball milling treatment, and modifying to obtain the required toughening agent;
the ball milling medium is a stainless steel ball with the diameter of 15 mu m, the ball-material ratio is 4:1, the ball milling rotating speed of the first time is 500r/min, the ball milling time is 2h, the ball milling rotating speed of the second time is 250r/min, and the ball milling time is 1.5h.
Preparation example 3
The toughening agent is prepared by the following method:
controlling the mass ratio of graphene oxide (particle size of 50 μm), liquid sodium silicate (modulus of 3.5) and silane coupling agent KH-550 to be 1:0.3:0.1, mixing the graphene oxide with the liquid sodium silicate, performing a first ball milling treatment, adding the silane coupling agent KH-550, performing a second ball milling treatment, and modifying to obtain the required toughening agent;
stainless steel balls with the diameter of 20 mu m are selected as the ball milling medium, the ball-material ratio is 4:1, the ball milling rotating speed of the first time is 600r/min, the ball milling time is 1h, the ball milling rotating speed of the second time is 200r/min, and the ball milling time is 2h.
Comparative preparation example 1
The toughening agent is prepared by the following method:
controlling the mass ratio of graphene oxide (particle size of 30 mu m), liquid sodium silicate (modulus of 3.2) and silane coupling agent KH-560 to be 1:0.2:0.1, mixing the graphene oxide with the liquid sodium silicate, performing first ball milling treatment, adding the silane coupling agent KH-560, performing second ball milling treatment, and modifying to obtain the required toughening agent;
the ball milling medium is a stainless steel ball with the diameter of 10 mu m, the ball-material ratio is 3:1, the ball milling rotating speed of the first time is 400r/min, the ball milling time is 3h, the ball milling rotating speed of the second time is 300r/min, and the ball milling time is 1h.
Comparative preparation example 2
The toughening agent is prepared by the following method:
controlling the mass ratio of graphene oxide (particle size of 30 mu m) to silane coupling agent KH-792 to be 1:0.1, performing first ball milling treatment on the graphene oxide, adding silane coupling agent KH-792, performing second ball milling treatment, and modifying to obtain the required toughening agent;
the ball milling medium is a stainless steel ball with the diameter of 10 mu m, the ball-material ratio is 3:1, the ball milling rotating speed of the first time is 400r/min, the ball milling time is 3h, the ball milling rotating speed of the second time is 300r/min, and the ball milling time is 1h.
Preparation examples 4-6 and comparative preparation examples 3-5 provide a multi-element alloy micropowder and a preparation method thereof.
Preparation example 4
The multi-element alloy micro powder comprises the raw materials of 8.2 percent of Mo, 2.3 percent of Ni, 0.5 percent of V, 0.2 percent of Co, 0.01 percent of Re and the balance of Mn in percentage by weight;
the preparation method comprises the following steps:
(1) Weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinding machine together, controlling the grinding pressure to be 60kPa, the grinding rotating speed to be 20r/min, and grinding for 70min to uniformly mix to obtain nano mixed powder;
(2) Adding a modifier into the nano mixed powder according to the mass ratio of 1:0.1, continuously grinding and mixing for 3 hours, then placing the mixture into the temperature of 380 ℃, and drying the mixture for 5 hours to obtain the needed multi-element alloy micro powder;
the modifier in the step (2) is a compound of methyl ethylene oxide and dodecanol in a mass ratio of 2:1.
Preparation example 5
The multi-element alloy micro powder comprises the raw materials of 10 percent of Mo, 3 percent of Ni, 0.6 percent of V, 0.25 percent of Co, 0.03 percent of Re and the balance of Mn in percentage by weight;
the preparation method comprises the following steps:
(1) Weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinding machine together, controlling the grinding pressure to be 70kPa, the grinding rotating speed to be 35r/min, and grinding for 50min to uniformly mix to obtain nano mixed powder;
(2) Adding a modifier into the nano mixed powder according to the mass ratio of 1:0.15, continuously grinding and mixing for 2 hours, then placing the mixture into the temperature of 420 ℃, and drying the mixture for 4 hours to obtain the needed multi-element alloy micro powder;
the modifier in the step (2) is a compound of methyl ethylene oxide and dodecanol in a mass ratio of 2.5:1.
Preparation example 6
The multi-element alloy micro powder comprises 13.5 weight percent of Mo, 4.4 weight percent of Ni, 0.8 weight percent of V, 0.3 weight percent of Co, 0.05 weight percent of Re and the balance of Mn;
the preparation method comprises the following steps:
(1) Weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinding machine together, controlling the grinding pressure to be 80kPa, the grinding rotating speed to be 50r/min, and grinding for 30min to uniformly mix to obtain nano mixed powder;
(2) Adding a modifier into the nano mixed powder according to the mass ratio of 1:0.2, continuously grinding and mixing for 1h, and then placing the mixture into the temperature of 460 ℃ for drying treatment for 3h to obtain the needed multi-element alloy micro powder;
the modifier in the step (2) is a compound of methyl ethylene oxide and dodecanol in a mass ratio of 3:1.
Comparative preparation example 3
The multi-element alloy micro powder comprises the raw materials of 8.2 percent of Mo, 2.3 percent of Ni, 0.5 percent of V, 0.2 percent of Co, 0.01 percent of Re and the balance of Mn in percentage by weight;
the preparation method comprises the following steps:
(1) Weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinding machine together, controlling the grinding pressure to be 60kPa, the grinding rotating speed to be 20r/min, and grinding for 70min to uniformly mix to obtain nano mixed powder;
(2) Adding methyl epoxy ethane into the nano mixed powder according to the mass ratio of 1:0.1, continuously grinding and mixing for 3 hours, then placing the mixture into the temperature of 380 ℃, and drying the mixture for 5 hours to obtain the needed multi-element alloy micro powder.
Comparative preparation example 4
The multi-element alloy micro powder comprises the raw materials of 8.2 percent of Mo, 2.3 percent of Ni, 0.5 percent of V, 0.2 percent of Co, 0.01 percent of Re and the balance of Mn in percentage by weight;
the preparation method comprises the following steps:
(1) Weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinding machine together, controlling the grinding pressure to be 60kPa, the grinding rotating speed to be 20r/min, and grinding for 70min to uniformly mix to obtain nano mixed powder;
(2) Adding dodecanol into the nano mixed powder according to the mass ratio of 1:0.1, continuously grinding and mixing for 3 hours, and then placing the mixture into the temperature of 380 ℃ for drying treatment for 5 hours to obtain the needed multi-element alloy micro powder.
Comparative preparation example 5
The multi-element alloy micro powder comprises the raw materials of 8.2 percent of Mo, 2.3 percent of Ni, 0.5 percent of V, 0.2 percent of Co, 0.01 percent of Re and the balance of Mn in percentage by weight;
the preparation method comprises the following steps:
weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinding machine, controlling the grinding pressure to be 60kPa, the grinding rotating speed to be 20r/min, the grinding time to be 250min, grinding and mixing uniformly, and then placing the mixture into the temperature of 380 ℃ for drying treatment for 5h to obtain the required multi-element alloy micro powder.
Examples 1-3 provide a composite coating applied to dental plate molds and a method of making the same.
Example 1
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm), polyimide (particle size 30 μm) and 30% by mass of polyvinyl alcohol aqueous solution in a mass ratio of 5:1:0.1;
the toughening agent is prepared in preparation example 1;
the multi-element alloy micropowder is prepared in preparation example 4.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Example 2
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 110 parts of resin composition, 4 parts of toughening agent and 10 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle diameter 20 mu m), polyimide (particle diameter 20 mu m) and polyvinyl alcohol aqueous solution with mass fraction of 20% in a mass ratio of 6:1:0.2;
the toughening agent is prepared in preparation example 2;
the multi-element alloy micropowder is prepared from preparation example 5.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 80 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.7MPa, the distance between the nozzle and the dental plate die is 26mm, and the sand blasting angle is 70 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 30min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring rotation speed to be 450r/min, and stirring and mixing for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 20mm, controlling the moving speed of a spray gun to be 25mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 1.5h in a vacuum environment at the temperature of 250 ℃ to obtain the required composite coating.
Example 3
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 120 parts of resin composition, 5 parts of toughening agent and 12 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 30 μm), polyimide (particle size 10 μm) and 10% by mass of polyvinyl alcohol aqueous solution in a mass ratio of 8:1:0.3;
the toughening agent is prepared in preparation example 3;
the multi-element alloy micropowder is prepared from preparation example 6.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 100 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.8MPa, the distance between the nozzle and the dental plate die is 30mm, and the sand blasting angle is 80 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 40min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 500r/min, and stirring and mixing for 15min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 30mm, controlling the moving speed of a spray gun to be 28mm/S, controlling the lap joint amount of adjacent passes to be 2mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 1h at the temperature of 280 ℃ in a vacuum environment to obtain the required composite coating.
To verify the performance of the composite coatings prepared in examples 1-3 of the present application, the applicant set comparative examples 1-7, which are specifically as follows:
comparative example 1
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm), polytetrafluoroethylene (particle size 30 μm) and a polyvinyl alcohol aqueous solution with mass fraction of 30% in a mass ratio of 5:1:0.1;
the toughening agent is prepared in preparation example 1;
the multi-element alloy micropowder is prepared in preparation example 4.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Comparative example 2
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm) and polyimide (particle size 30 μm) in a mass ratio of 5:1;
the toughening agent is prepared in preparation example 1;
the multi-element alloy micropowder is prepared in preparation example 4.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Comparative example 3
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm), polyimide (particle size 30 μm) and 30% by mass of polyvinyl alcohol aqueous solution in a mass ratio of 5:1:0.1;
the toughening agent is prepared in comparative preparation example 1;
the multi-element alloy micropowder is prepared in preparation example 4.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Comparative example 4
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm), polyimide (particle size 30 μm) and 30% by mass of polyvinyl alcohol aqueous solution in a mass ratio of 5:1:0.1;
the toughening agent is prepared in comparative preparation 2;
the multi-element alloy micropowder is prepared in preparation example 4.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Comparative example 5
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm), polyimide (particle size 30 μm) and 30% by mass of polyvinyl alcohol aqueous solution in a mass ratio of 5:1:0.1;
the toughening agent is prepared in preparation example 1;
the multi-element alloy micropowder is prepared from comparative example 3.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Comparative example 6
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm), polyimide (particle size 30 μm) and 30% by mass of polyvinyl alcohol aqueous solution in a mass ratio of 5:1:0.1;
the toughening agent is prepared in preparation example 1;
the multi-element alloy micropowder is prepared from comparative example 4.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Comparative example 7
The composite coating applied to the dental plate die comprises the following raw materials in parts by weight: 100 parts of resin composition, 3 parts of toughening agent and 8 parts of multi-element alloy micro powder;
wherein the resin composition comprises polytetrafluoroethylene (particle size 10 μm), polyimide (particle size 30 μm) and 30% by mass of polyvinyl alcohol aqueous solution in a mass ratio of 5:1:0.1;
the toughening agent is prepared in preparation example 1;
the multi-element alloy micropowder is prepared from comparative example 5.
The preparation method of the composite coating applied to the dental plate die comprises the following preparation steps:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning, degreasing and impurity-removing the dental plate die, drying, and then carrying out sand blasting treatment, wherein white corundum micro powder with the particle size of 60 mu m is adopted for sand blasting, the outlet pressure of a nozzle of a sand blaster is 0.5MPa, the distance between the nozzle and the dental plate die is 20mm, and the sand blasting angle is 50 degrees, so that the dental plate die to be sprayed is obtained;
s3, pre-grinding and mixing the toughening agent and the multi-element alloy micro powder for 20min until the toughening agent and the multi-element alloy micro powder are uniformly mixed, adding the toughening agent and the multi-element alloy micro powder into the resin composition while stirring, controlling the stirring speed to be 400r/min, and stirring and mixing for 25min until the toughening agent and the multi-element alloy micro powder are uniformly mixed to obtain a composite coating raw material;
s4, controlling the spraying distance to be 18mm, controlling the moving speed of a spray gun to be 20mm/S, controlling the overlap joint amount of adjacent passes to be 1mm and the thickness of the composite coating to be 150 mu m, spraying the raw material of the composite coating on the surface of a die to be sprayed at room temperature, and curing for 2 hours at 220 ℃ in a vacuum environment to obtain the required composite coating.
Performance testing
The composite coatings of examples 1-3 and comparative examples 1-7 of the present application were prepared as test samples, respectively, and the properties of the composite coatings were tested as follows:
using a G200 nano indentation instrument to test hardness and elastic modulus, and specifically selecting a continuous stiffness method of the nano indentation instrument;
carrying out a scratch test by using a scratch tester, specifically sliding a Rockwell diamond needle on the surface of a composite coating sample at a speed of 1mm/min, increasing the load at a speed of 10N/min, and recording the load when the film layer of the composite coating sample is scratched, wherein the load is recorded as a critical load;
the UMT frictional wear testing machine is used for carrying out wear resistance test, and the friction control conditions are as follows: the friction pair is steel, the friction load is 10N, and the friction time is 2h;
the specific test results are shown in table 1 below:
table 1:
as can be seen from the data shown in table 1: the composite coating prepared in the embodiment 1-3 of the application has high hardness, low elastic modulus, high critical load value and low coating wear rate, namely the composite coating prepared in the embodiment 1-3 of the application has more excellent wear resistance, toughness and adhesive force compared with the comparative examples 1-7.
As can be seen from examples 1 and comparative examples 1 to 2, the resin composition is compounded with polytetrafluoroethylene, polyimide and aqueous polyvinyl alcohol solution, and the comprehensive performance of the finally prepared composite coating is obviously improved compared with the method of only selecting polytetrafluoroethylene and aqueous polyvinyl alcohol solution or not adding aqueous polyvinyl alcohol solution into the resin composition.
As is clear from example 1 and comparative examples 3 to 4, the liquid sodium silicate and the aminosilane coupling agent are used for sequentially modifying graphene oxide, so that the dispersibility, compatibility, stability, mechanical properties and the like of the graphene oxide can be remarkably improved, and the modified graphene oxide is used for formula addition, so that the adhesive force and toughness of the composite coating can be remarkably improved, and meanwhile, the hardness and wear resistance of the composite coating can be further enhanced.
As is clear from examples 1 and comparative examples 5 to 7, under the condition that other conditions are not changed, the composite coating can be further and remarkably improved in comprehensive performance by modifying the multi-element alloy micro powder by using methyl ethylene oxide and dodecanol together, compared with the method of independently selecting methyl ethylene oxide or dodecanol or directly modifying without using a modifier.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (6)
1. The composite coating applied to the dental plate die is characterized by comprising the following raw materials in parts by weight: 100-120 parts of resin composition, 3-5 parts of toughening agent and 8-12 parts of multi-element alloy micropowder;
the resin composition comprises polytetrafluoroethylene, polyimide and polyvinyl alcohol aqueous solution in a mass ratio of 5-8:1:0.1-0.3;
the toughening agent is prepared by mixing graphene oxide with liquid sodium silicate, and then modifying the mixture by silane;
the multi-element alloy micro powder comprises raw materials Mo, ni, V, co, re and Mn;
the toughening agent is prepared by the following method:
controlling the mass ratio of graphene oxide to liquid sodium silicate to silane coupling agent to be 1:0.2-0.3:0.1, mixing the graphene oxide with the liquid sodium silicate, performing first ball milling treatment, adding the silane coupling agent, performing second ball milling treatment, and modifying to obtain the required toughening agent;
the silane coupling agent is an aminosilane coupling agent;
the multi-element alloy micro powder comprises, by weight, 8.2-13.5% of Mo, 2.3-4.4% of Ni, 0.5-0.8% of V, 0.2-0.3% of Co, 0.01-0.05% of Re and the balance Mn;
the multi-element alloy micro powder is prepared by the following method:
(1) Weighing raw materials Mo, ni, V, co, re and Mn according to weight percentage, adding the raw materials into a grinder together, and grinding and mixing uniformly to obtain nano alloy powder;
(2) Adding modifier into the nano mixed powder according to the mass ratio of 1:0.1-0.2, continuously grinding and mixing for 1-3h, and drying to obtain the needed multi-element alloy micro powder;
the modifier in the step (2) is a compound of methyl ethylene oxide and dodecanol in a mass ratio of 2-3:1.
2. The composite coating applied to a dental plate mold according to claim 1, comprising the following raw materials in parts by weight: 110 parts of resin composition, 4 parts of toughening agent and 10 parts of multi-element alloy micropowder.
3. The composite coating applied to a dental plate mold according to claim 1, wherein the first ball milling speed is 400-600r/min and the ball milling time is 1-3h; the second ball milling rotating speed is 200-300r/min, and the ball milling time is 1-2h.
4. The composite coating applied to a dental plate mold according to claim 1, wherein the grinding pressure in the step (1) is 60-80kPa, the grinding rotation speed is 20-50r/min, and the grinding time is 30-70min.
5. The composite coating applied to a dental plate mold according to claim 1, wherein the drying temperature in the step (2) is 380-460 ℃ and the drying time is 3-5h.
6. A method of preparing a composite coating for dental plate molds according to any one of claims 1 to 5, comprising the steps of:
s1, weighing a raw material resin composition, a toughening agent and multi-element alloy micro powder according to parts by weight for standby;
s2, cleaning and drying the dental plate die, and then performing sand blasting treatment to obtain the dental plate die to be sprayed;
s3, after premixing the toughening agent and the multi-element alloy micro powder uniformly, adding the toughening agent and the multi-element alloy micro powder into the resin composition, and stirring and mixing uniformly to obtain a composite coating raw material;
and S4, spraying the composite coating raw material on the surface of the die to be sprayed, and carrying out vacuum curing to obtain the required composite coating.
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