CN115609184B - Modified tin powder, preparation method thereof and tin paste - Google Patents
Modified tin powder, preparation method thereof and tin paste Download PDFInfo
- Publication number
- CN115609184B CN115609184B CN202211635961.0A CN202211635961A CN115609184B CN 115609184 B CN115609184 B CN 115609184B CN 202211635961 A CN202211635961 A CN 202211635961A CN 115609184 B CN115609184 B CN 115609184B
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- tin powder
- group
- adhesion layer
- compound
- modified
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 232
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- 239000000843 powder Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
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- 125000004423 acyloxy group Chemical group 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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Abstract
The invention relates to the technical field of welding, in particular to modified tin powder, a preparation method thereof and tin paste. The modified tin powder comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the raw material of the first adhesion layer comprises a disilane compound, and the disilane compound is subjected to polycondensation to form a silane compound containing a silicon-oxygen group so as to form the first adhesion layer. The modified tin powder provided by the invention has good surface performance, good dispersibility in tin paste and difficult agglomeration.
Description
Technical Field
The invention relates to the technical field of welding, in particular to modified tin powder, a preparation method thereof and tin paste.
Background
Solder paste is a paste-like material used to solder electronic components on a base or a circuit board to prevent the electronic components from shifting under vibration. The solder paste generally comprises two parts of soldering flux and solder powder, wherein the solder powder mainly comprises various metal alloy particles, and the soldering flux contains a solvent for mixing various additives and the solder powder together. With the miniaturization of electronic parts and the rapid development of Mini LEDs or Micro LEDs, the requirement of ultra-fine pitch is often met by adopting tin powder with smaller particle size, but greater challenges are provided for welding electronic parts on a printed circuit board. The solder paste prepared by the existing fine solder powder is easy to have the problems of grape-shaped welding, continuous tin and other welding defects. The above problems arise because: firstly, the surface of the powder is enlarged due to the adoption of finer tin powder, a large amount of tin powder is easier to oxidize, and the prepared tin paste has the phenomenon of serious agglomeration and difficult dispersion; secondly, the acting force of the soldering flux on the powder is lower, so that the tin powder is more prone to sedimentation after agglomeration. Moreover, the problem of dispersion of the solder powder becomes more serious with time, and the thickening of the solder paste is not sufficiently suppressed, which results in a shortened effective time of the solder paste. In addition, the solder paste has the problems of nozzle blockage caused by poor fluidity in the spray printing process, and the collapse of the solder paste after spray printing due to poor uniformity of all components in the solder paste.
Disclosure of Invention
The technical problem to be solved by the invention is to provide modified tin powder which has good surface property, good dispersibility in tin paste and difficult agglomeration.
The technical problem to be solved by the invention is also to provide a preparation method of the in-vitro modified tin powder, which is simple in process and suitable for large-scale production.
In order to solve the technical problem, the invention provides modified tin powder, which comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the raw material of the first adhesion layer comprises a disilane compound, and the disilane compound is condensed to form a silane compound containing a silicon-oxygen group so as to form the first adhesion layer.
In one embodiment, the raw material of the first adhesion layer comprises a disilane compound and a monosilane compound, which are condensed to form a silane-based compound containing a siloxy group to form the first adhesion layer;
the monosilane compound or the disilane compound contains one or more of alkoxy, halogen group, acyloxy and amino in the structure.
In one embodiment, the monosilane compound has the molecular structure (i):
the molecular structural formula (I) is as follows:
the molecular structural formula of the bis-silane compound is (II), (III) or (IV):
the molecular structural formula (II) is as follows:
the molecular structural formula (III) is as follows:
the molecular structural formula (IV) is as follows:
wherein, R is 1 、R 2 Or R 3 Is one of alkyl group, alkenyl group, phenyl group, amino group, halogen group, sulfhydryl group and hydrogen group;
the X is one of alkoxy, halogen group, acyloxy and amino;
a is one of alkyl, alkoxy, halogen group, acyloxy and amino;
b is one of alkyl, alkoxy, halogen group, acyloxy and amino;
m≥0，n≥0。
preferably, said R is 1 Is an alkenyl group;
x, A and B are both alkoxy;
0≤m≤10，0≤n≤10。
more preferably, the X, A, B has the same molecular structural formula;
the alkoxy is one or more of methoxy, ethoxy, propoxy and isopropoxy;
1≤m≤3，1≤n≤3。
preferably, the monosilane compound is one selected from methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, vinyltriethoxysilane, propyltrichlorosilane, butyltrichlorosilane, p-tolyltrimethoxysilane, (3-aminopropyl) triethoxysilane, and (3-mercaptopropyl) trimethoxysilane;
the disilane compound is one of bis (triethoxysilyl) methane, 1,2-bis (trimethoxysilyl) ethane, 1,2-bis (trimethoxysilyl) decane, bis- [3- (triethoxysilyl) propyl ] -disulfide and bis- [3- (triethoxysilyl) propyl ] -tetrasulfide.
In one embodiment, the raw material of the first adhesion layer comprises a monosilane compound and a disilane compound, the monosilane compound: the mass ratio of the disilane compound is 1: (0.1-0.6);
the number of molecular layers of the first adhesion layer is 5-20 layers;
the thickness of the first adhesion layer is 0.1-0.4 μm.
In one embodiment, the tin powder particles further comprise a second adhesion layer coated on the outer surface of the first adhesion layer, and the second adhesion layer is a polymer containing amide groups.
In one embodiment, the molecular structure of the second attachment layer is (v):
the molecular structural formula (V) is:
wherein, R is 4 、R 5 Or R 6 Is one of hydrogen radical or alkyl;
the R is 7 Is one or more of hydrogen group, alkyl group, hydroxyl group, ether group and phenyl group;
the above-mentionedl≥3。
Preferably, said R is 7 Is alkyl hydroxyl or alkyl ether;
5≤l≤15。
more preferably, the monomer corresponding to the second adhesion layer polymer is one selected from the group consisting of acrylamide, methacrylamide, N-ethylacrylamide, N-isopropylacrylamide, N-tert-butylacrylamide, N-isopropylmethacrylamide, N-methylolacrylamide, N-hydroxyethylacrylamide, N- [ tris (hydroxymethyl) methyl ] acrylamide, N- (butoxymethyl) acrylamide, N- (isobutoxymethyl) acrylamide, and N-phenylacrylamide.
In order to solve the problems, the invention also provides a preparation method of the modified tin powder, which comprises the following steps:
cleaning the tin powder particles to obtain first tin powder particles;
mixing a monosilane compound and/or a disilane compound with an alcohol substance and water to prepare a first mixed solution;
and adding the first tin powder particles into the first mixed solution, stirring for a preset time, and drying to obtain a finished product.
In addition, the invention also provides another preparation method of the modified tin powder, which comprises the following steps:
cleaning the tin powder particles to obtain first tin powder particles;
mixing a monosilane compound and/or a disilane compound with an alcohol substance and water to prepare a first mixed solution;
adding the first tin powder particles into the first mixed solution, stirring for a preset time, and drying to obtain first modified tin powder;
and adding the first modified tin powder into the polymer containing the amide group, stirring for a preset time, and drying to obtain a finished product.
Correspondingly, the invention also provides a solder paste which comprises the modified solder powder and the soldering flux.
In one embodiment, the soldering flux comprises an auxiliary agent, wherein the auxiliary agent is one or more of ethyl acetate, methyl acetate and dimethyl malonate;
the mass ratio of the modified tin powder to the auxiliary agent is 40: (0.5-1);
the modified tin powder accounts for 80-90% of the total mass of the tin paste.
The implementation of the invention has the following beneficial effects:
the modified tin powder provided by the invention comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the first adhesion layer is a silane compound containing a silicon-oxygen group. The first adhesion layer can reduce the oxidation of the tin powder before the preparation of the tin paste, and improve the use reliability of the tin paste. In addition, the first adhesion layer can improve the surface performance of the tin powder particles, improve the dispersion capability of the tin powder particles in the tin paste and reduce agglomeration. In addition, when the first adhesion layer containing a siloxane-based silane compound is formed, curing shrinkage occurs, and additional stress is generated on the surface of the tin powder particles, thereby securing the degree of bonding between the first adhesion layer and the tin powder particles.
Furthermore, the tin powder particles also comprise a second adhesion layer outside, the second adhesion layer is coated on the outer surface of the first adhesion layer, and the second adhesion layer is a polymer containing amide groups. The second adhesion layer enables the modified tin powder and the soldering flux to appropriately coexist, and further meets the application characteristics of the tin paste. The second adhesion layer is a polymer containing amide groups, and a large number of amide groups can form chemical bonds with various components in the soldering flux through nucleophilic or adsorption action, even form hydrogen bonds with macromolecular compounds in the soldering flux, and serve as bridges for tin powder and soldering flux solution, so that the dispersibility of the tin powder in tin paste is improved.
The invention provides a solder paste which adopts the modified solder powder and the soldering flux, has good dispersibility, uniform texture and strong stability, is not easy to agglomerate and can meet the requirement of hyperfine spacing. Moreover, the problems of welding defects such as grape-shaped welding, continuous tin and the like can be effectively avoided, and the nozzle is not easy to block due to good fluidity in the spray printing process.
Drawings
FIG. 1 is a graphical illustration for characterizing the performance of solder powder in solder paste applications.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
Unless otherwise stated or contradicted, terms or phrases used herein have the following meanings:
in the present invention, the terms "combination thereof", "any combination thereof", and the like include all suitable combinations of any two or more of the listed items.
In the present invention, "preferred" is only an embodiment or an example for better description, and it should be understood that the scope of the present invention is not limited thereto.
In the present invention, the technical features described in the open type include a closed technical solution composed of the listed features, and also include an open technical solution including the listed features.
In the present invention, the numerical range is defined to include both end points of the numerical range unless otherwise specified.
In order to solve the technical problem, the invention provides modified tin powder, which comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the raw material of the first adhesion layer comprises a disilane compound, and the disilane compound is condensed to form a silane compound containing a silicon-oxygen group so as to form the first adhesion layer.
The modified tin powder provided by the invention comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the first adhesion layer is a silane compound containing a silicon-oxygen group. The first adhesion layer can reduce the oxidation of the tin powder before the preparation of the tin paste, and improve the use reliability of the tin paste. In addition, the first adhesion layer can improve the surface performance of the tin powder particles, improve the dispersion capacity of the tin powder particles in the tin paste and reduce agglomeration. In addition, when the first adhesion layer containing a siloxane-based silane compound is formed, curing shrinkage occurs, and additional stress is generated on the surface of the tin powder particles, thereby securing the degree of bonding between the first adhesion layer and the tin powder particles.
In one embodiment, the raw material of the first adhesion layer comprises a disilane compound and a monosilane compound, which are condensed to form a silane-based compound containing a siloxy group to form the first adhesion layer. In the present invention, the monosilane compound refers to a compound having a single silicon-based functional group, and the disilane compound refers to a compound having two silicon-based functional groups. In one embodiment, the monosilane compound or the disilane compound contains one or more of an alkoxy group, a halogen group, an acyloxy group, and an amino group in the structure. The above groups may be hydrolyzed to form silanols, and then dehydrated to form a polycondensate containing silicon oxy groups after condensation of hydroxyl groups between the silanols and attached to the surface of the tin powder particles.
In one embodiment, the monosilane compound or the disilane compound has a structure containing one or more of an alkoxy group, a halogen group, an acyloxy group, and an amino group.
In one embodiment, the monosilane compound has the molecular structural formula (i):
the molecular structural formula (I) is as follows:
the molecular structural formula of the bis-silane compound is (II), (III) or (IV):
the molecular structural formula (II) is as follows:
the molecular structural formula (III) is as follows:
the molecular structural formula (IV) is as follows:
wherein, R is 1 、R 2 Or R 3 Is one of alkyl group, alkenyl group, phenyl group, amino group, halogen group, sulfhydryl group and hydrogen group;
the X is one of alkoxy, halogen group, acyloxy and amino;
a is one of alkyl, alkoxy, halogen group, acyloxy and amino;
b is one of alkyl, alkoxy, halogen group, acyloxy and amino;
m≥0，n≥0。
according to the invention, the monosilane compound and/or the disilane compound are condensed to form the first adhesion layer, the first adhesion layer is the silane compound containing siloxy, so that bare tin powder particles and soldering flux are isolated, and meanwhile, the wetting property between the tin powder and the soldering flux is improved by virtue of the condensation polymer. The disilane compound has stronger polymerization capacity, particularly when A, B and X are all hydrolysable groups, the disilane compound has the capacity of six bonds, the crosslinking density can be effectively improved, a more compact adhesive layer crosslinking network can be formed, the bonding force with tin powder particles is firmer, the stability of the modified tin powder in the tin paste is further improved, and the storage time of the tin paste can be further prolonged.
However, when the disilane compound is used only or the ratio of the disilane compound is too large, the tolerance of the modified tin powder is too large, which affects the reaction conditions of the tin powder during reflow soldering and the wettability of the tin paste during soldering, and the phenomenon of tin beading or tin bridging caused by the solder paste escaping from the pad may be aggravated as the printing time is prolonged. Thus, in one embodiment, the starting material of the first adhesion layer comprises a monosilane compound and a disilane compound, the monosilane compound: the mass ratio of the disilane compound is 1: (0.1-0.6). Preferably, the monosilane compound: the mass ratio of the disilane compound is 1: (0.2-0.3).
Specifically, R in the molecular structural formula of the monosilane compound 1 And the alkyl group is one of methyl, ethyl, propyl, tert-butyl and isopropyl. Preferably, R 1 The groups are ethyl, propyl and tert-butyl, and have proper carbon chain length, so that the stability of the silane compound and the compactness of an adhesive layer coated by tin powder can be ensured. The alkenyl group includes a vinyl group. The phenyl group is selected from one of phenyl, p-tolyl and iso-tolyl. The amino group includes an aminoethyl group or an aminopropyl group. The halogen group comprises chloromethyl or chloropropyl. The mercapto group-like group includes mercaptopropyl. More preferably, R 1 The groups are alkenyl groups. In order to realize the coating effect of the first adhesion layer and the tin powder surface,the bonding ability or adsorption ability of the monosilane compound or the disilane compound used for the adhesion layer to the surface of the tin powder needs to be considered. In general, R 1 The groups affect the performance of the silane compound at the critical plane, and the tin powder can be wetted when the monosilane compound or the disilane compound has a surface tension lower than that of the tin powder at the critical plane. R 1 The surface tension of the coating solution can be reduced by the alkenyl group, the tin powder surface can be soaked more easily, and the stronger the soaking effect, the stronger the adsorption capacity can be presented.
In the molecular structural formula for the bis-silane compoundmValue (c),nThe longer the carbon chain, the more the formed crosslinked network adhesion layer may extend from the surface of the tin powder, but in view of ease of synthesis and coating effect of the formed adhesion layer, it is preferable that 0. Ltoreq. M.ltoreq. 10,0. Ltoreq. N.ltoreq.10. More preferably, m is more than or equal to 1 and less than or equal to 3,1 and less than or equal to 3.
Regarding X, A and B in the molecular structural formulas of the monosilane compound and the disilane compound, in one embodiment, X, A, B is a hydrolyzable group, i.e., at least one of alkoxy, halogen, acyloxy, and amino. Thus, the condensation difficulty can be reduced, and the efficiency of the modification process can be improved. For example, the X group is hydrolyzed to form alcoholic hydroxyl group, which can rapidly react with the alcoholic hydroxyl group of the A group or the B group of other silane compounds to form silane compounds. And, the hydrolyzable group not participating in the condensation process, which may exist as the formation of alcoholic hydroxyl group after the silane-based compound is formed, may form chemical covalent interaction or other physical interaction with the soldering flux in the subsequent solder paste preparation process. Preferably, the X, A and B are both alkoxy groups. More preferably, the X, A, B has the same molecular structural formula; the alkoxy is one or more of methoxy, ethoxy, propoxy and isopropoxy; this helps to provide a regular arrangement of chemical groups in the adhesion layer formed, which helps to improve the uniformity of tin powder distribution in the flux.
In one embodiment, at least one of the X, A, B is methoxy or ethoxy. The methoxy and ethoxy have low requirements on conditions in the polycondensation process for forming the silane compound, and the polycondensation reaction is easier to occur; and the first adhesion layer formed by the methoxyl group or/and the ethoxyl group has stronger adhesive force with the tin powder particles, and has better stability in the tin paste.
Preferably, the monosilane compound is selected from one of methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, vinyltriethoxysilane, propyltrichlorosilane, butyltrichlorosilane, p-tolyltrimethoxysilane, (3-aminopropyl) triethoxysilane, and (3-mercaptopropyl) trimethoxysilane;
the disilane compound is one of bis (triethoxysilyl) methane, 1,2-bis (trimethoxysilyl) ethane, 1,2-bis (trimethoxysilyl) decane, bis- [3- (triethoxysilyl) propyl ] -disulfide and bis- [3- (triethoxysilyl) propyl ] -tetrasulfide.
The specific compounds listed above are capable of achieving the objects of the present invention well in view of the above-mentioned processes of action taken together.
Finally, theoretically, if a completely dense single molecular layer can be formed on the surface of the tin powder, the isolation effect can be satisfied. However, due to the material characteristics of the silane compounds and the comprehensive consideration of the coating quality, if the number of molecular layers is too small or the thickness is too low, the compactness of the coated tin powder is insufficient, the requirement of the oxygen content on the surface of the tin powder cannot be met, and the stability and the dispersibility after the tin paste is prepared are poor. If the number of the molecular layers is too large or the thickness is too large, the most direct influence is that the original particle size and the particle size distribution of the tin powder are changed, and particularly the movement of the spray type tin paste in a nozzle is influenced; in addition, the molecular layer number or thickness of the adhesive layer on the surface of the tin powder can also cause the problem that the adhesive layer of the prepared tin paste is not easy to fall off or remove in the welding process, thereby interfering the service performance of the tin paste. And the proper thickness is more friendly to the reaction condition of the solution method or the spraying method by combining the preparation process. In one embodiment, the first adhesion layer has a molecular layer number of 5 to 20 layers; the thickness of the first adhesion layer is 0.1-0.4 μm. The adhesive layer with the molecular layer number or the thickness can form a relatively ideal cross-linked network structure on the surface of the tin powder so as to meet the requirements of the modified tin powder and the prepared tin paste in various aspects.
Further, in an embodiment, the tin powder particles further include a second adhesion layer, the second adhesion layer is coated on the outer surface of the first adhesion layer, and the second adhesion layer is a polymer containing an amide group.
The second adhesion layer enables the modified tin powder and the soldering flux to appropriately coexist, and further meets the application characteristics of the tin paste. The second adhesion layer is a polymer containing amide groups, and a large number of amide groups can form chemical bonds with various components in the soldering flux through nucleophilic or adsorption action, even form hydrogen bonds with macromolecular compounds in the soldering flux, and serve as bridges for tin powder and soldering flux solution, so that the dispersibility of the tin powder in tin paste is improved.
In one embodiment, the molecular structure of the second attachment layer is (v):
the molecular structural formula (V) is:
wherein, R is 4 、R 5 Or R 6 Is one of hydrogen radical or alkyl;
the R is 7 Is one or more of hydrogen group, alkyl group, hydroxyl group, ether group and phenyl group;
the describedl≥3。
Wherein R is 7 The group belongs to a substituent on N, and the functional group of the substituent can change the acting force of the coating layer and macromolecular compounds (such as rosin) in the solder paste soldering flux. Preferably, said R is 7 Is alkyl hydroxyl or alkyl ether. By controlling the degree of polymerization or molecular weight of the polymer, the solubility characteristics of the formed second adhesive layer in the flux can be adjusted. Preferably, 5. Ltoreql≤15。
More preferably, the monomer corresponding to the second adhesion layer polymer is one of acrylamide, methacrylamide, N-ethylacrylamide, N-isopropylacrylamide, N-tert-butylacrylamide, N-isopropylmethacrylamide, N-methylolacrylamide, N-hydroxyethylacrylamide, N- [ tris (hydroxymethyl) methyl ] acrylamide, N- (butoxymethyl) acrylamide, N- (isobutoxymethyl) acrylamide, and N-phenylacrylamide.
In order to solve the problems, the invention also provides a preparation method of the modified tin powder, which comprises the following steps:
s1, cleaning tin powder particles to obtain first tin powder particles;
in one embodiment, performing the cleaning of the tin powder particles includes: and pouring the bare tin powder into a low-concentration acid solution for acidity, washing the bare tin powder for multiple times by using ethanol or water, and drying the bare tin powder.
It should be noted that the step of pickling the tin powder is not necessary, and the tin powder may be washed with water or directly coated. Preferably, the tin powder is coated after the surface oxide layer is removed by acid cleaning, so that the coating effect is better, and the effect of removing the oxide layer is more ideal.
In one embodiment, the tin powder is selected from one or a combination of No. 5 tin powder, no. 6 tin powder or No. 7 tin powder, and the method can be applied to tin powder with various fine particle sizes, such as average particle size below 20 μm.
S2, mixing a monosilane compound and/or a disilane compound with an alcohol substance and water to prepare a first mixed solution;
the alcohol substance is selected from ethanol or methanol; a small amount of acid, such as acetic acid, can be added to adjust the pH value of the solution; in one embodiment, the first mixed solution is prepared from, by weight, 2 to 8 parts of the monosilane compound and/or the disilane compound, 2 to 96 parts of the alcohol substance, and 2 to 96 parts of water. In addition, for silane compounds that are difficult to dissolve in a solvent, a small amount of a modifier, such as an emulsion, may be added.
And S3, adding the first tin powder particles into the first mixed solution, stirring for a preset time, and drying to obtain a finished product.
In one embodiment, the drying temperature is from 25 ℃ to 150 ℃; the preset time is 3min-48h.
The first adhesion layer is coated outside the prepared modified tin powder, and the preparation method of the first adhesion layer and the second adhesion layer coated outside the modified tin powder comprises the following steps:
the invention also provides another preparation method of the modified tin powder, which comprises the following steps:
s1, cleaning tin powder particles to obtain first tin powder particles;
s2, mixing a monosilane compound and/or a disilane compound with an alcohol substance and water to prepare a first mixed solution;
s3, adding the first tin powder particles into the first mixed solution, stirring for a preset time, and drying to obtain first modified tin powder;
and S4, adding the first modified tin powder into the amide group-containing polymer, stirring for a preset time, and drying to obtain a finished product.
The preparation method is to prepare the modified tin powder by a solution method, and in addition, the modified tin powder can be prepared by an atomization method. The atomization method is realized by introducing steam of reactants into atomization reaction equipment; the atomization device can adopt a pressure gas atomization device and a centrifugal atomization device; the atomization cavity contains inert gas which can be nitrogen, helium, argon or the like. The steam may be reduced in pressure.
Correspondingly, the invention also provides a solder paste which comprises the modified solder powder and the soldering flux. In one embodiment, the soldering flux comprises an auxiliary agent, wherein the auxiliary agent is one or more of ethyl acetate, methyl acetate and dimethyl malonate; the mass ratio of the modified tin powder to the auxiliary agent is 40: (0.5-1); the modified tin powder accounts for 80-90% of the total mass of the tin paste.
It should be noted that, in the process of forming the adhesion layer on the surface of the tin powder, the silane solution is converted into a compound with a large number of hydroxyl groups through hydrolysis, the ester auxiliary agent can form a certain combined action with the hydroxyl groups through the functional groups, and a hydrophobic protective film is added on the surface of the tin powder or the adhesion layer to a certain extent, which is equivalent to the action of the corrosion inhibitor.
Meanwhile, because the soldering flux of the tin paste contains various compounds such as alcohols, acids, ethers, phenols, esters, rosin and the like, the adhesive layer of the tin powder can be corroded in the tin paste, and the auxiliary agent is added to cooperate with the adhesive layer on the surface of the tin powder particles for protection, so that the stability of the tin powder particles in the soldering flux is improved.
In one embodiment, the flux is selected from one or a combination of thixotropic agents, active agents, antioxidants, film formers, and solvents. The thixotropic agent comprises hydrogenated castor oil or polyamide wax, the active agent is selected from one or combination of adipic acid, malonic acid and phthalic acid, and the antioxidant is selected from hydroquinone and/or catechol; the film forming agent comprises modified rosin; the solvent comprises terpineol and/or triethylene glycol monoethyl ether.
The invention is further illustrated by the following specific examples:
example set 1
The group of embodiments provides a modified tin powder, which comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the raw material of the first adhesion layer comprises a disilane compound and a monosilane compound, and the disilane compound and the monosilane compound are condensed to form a silane compound containing a siloxy group so as to form the first adhesion layer.
Table 1 shows the mass ratio of the monosilane compound to the disilane compound in example group 1
The preparation method of the modified tin powder comprises the following steps:
s1, cleaning tin powder particles to obtain first tin powder particles; wherein, no. 7 tin powder is adopted, and is dried after primary acid washing, secondary acid washing and water washing in sequence.
S2, mixing 3 parts of monosilane compound and/or disilane compound with 5 parts of anhydrous ethanol and 92 parts of water according to parts by weight to prepare a first mixed solution; wherein the monosilane compound is ethyltrimethoxysilane, and the disilane compound is 1,2-bis (trimethoxysilylo) ethane. In addition, in the preparation method of comparative example 1, the first mixed solution was mixed of only 5 parts of anhydrous ethanol and 92 parts of water.
And S3, adding 10g of the first tin powder particles into 200mg of the first mixed solution, stirring for 2h, and drying at 50 ℃ to obtain the modified tin powder.
And finally, adding an auxiliary agent and a soldering flux into the modified tin powder, wherein the auxiliary agent is ethyl acetate to prepare the tin paste, the modified tin powder accounts for 85% of the total mass of the tin paste, and the mass ratio of the modified tin powder to the auxiliary agent is 40:0.5.
the modified tin powder or tin paste obtained in the examples 1-1 to 1-9 and the comparative example 1 is tested, and the test items and the method are as follows:
(1) Oxygen content
And (3) placing the modified tin powder in a drying box at 35 ℃ for 48h, and testing the oxygen contents of the surfaces of the naked tin powder particles and the modified tin powder by an oxygen-nitrogen testing instrument so as to represent the coating effect of the tin powder. The higher the oxygen content is, the less effective the coating effect of the adhesion layer is, and the tin powder cannot be completely isolated from being oxidized.
(2) Dispersibility
And (3) testing by adopting a spectrophotometry method, pouring tin powder particles with the same mass into a test solution, taking the supernatant of the tin powder particles as a test sample after stirring, testing the absorbance of the sample, and comparing the dispersion performance among the samples according to the absorbance so as to represent the dispersion performance of the tin powder, wherein the lower the absorbance is, the more serious the agglomeration problem of the sample is, the shorter the suspension time in the solution is, and the poorer the dispersion performance is.
(3) Tin bead test
Referring to the industry standard JIS Z3284, the prepared solder paste was melted, cooled to room temperature, printed on a substrate that could not be wetted with solder, subjected to morphological observation and statistical analysis using a magnifying glass of a certain magnification, and evaluated according to the following table and fig. 1. Therefore, the service performance of the tin powder in the application of the tin paste is represented.
(4) Adhesion Change test
And placing the prepared solder paste in a 30 ℃ thermostat, and measuring the change condition of the adhesive strength of the sample after the solder paste is placed for one week so as to represent the stability of the solder paste. A large change in adhesion indicates a more serious problem with agglomeration of the sample during storage.
(5) Reflow testing
The prepared solder paste is subjected to screen printing through steel nets with different mesh point diameters (such as 0.20mm, 0.22mm, 0.24mm, 0.26mm, 0.28mm and 0.30 mm), the solder paste is subjected to shape observation after a reflow furnace, and the minimum mesh point diameter allowed by the solder paste when the solder paste avoids grape-shaped welding points is evaluated, so that the application effect of the solder powder containing the adhesive layer in the solder paste is represented.
The results of the above tests on the modified solder powders or pastes obtained in examples 1-1 to 1-9 and comparative example 1 are shown in Table 2:
table 2 shows the results of the performance tests of the modified tin powders or pastes of examples 1 to 1
From the above results, it can be seen that the content of the disilane compound is too low, the oxygen content is higher, the dispersibility during storage is poor, the change of the adhesion degree is large, and the reflow soldering test effect is general. The content of the disilane compound is too high, and the reflow soldering performance is poor. In the above table, the most suitable way for the production application is in examples 1-4.
The group of embodiments provides a modified tin powder, which comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the raw materials of the first adhesion layer comprise a disilane compound and a monosilane compound, and the disilane compound and the monosilane compound are subjected to condensation polymerization to form a silane compound containing a siloxane group so as to form the first adhesion layer.
Table 2 shows the chemical compositions of the monosilane compound and the disilane compound in example group 1
Referring to example group 1, the first mixed solution is prepared by mixing 5 parts of monosilane compound and/or disilane compound, 5 parts of anhydrous ethanol and 90 parts of water; and the mass ratio of the monosilane compound to the disilane compound is 1.
The test results of the modified solder powders or solder pastes obtained in examples 2-1 to 2-14 are shown in Table 3:
table 3 shows the results of the performance tests of the modified tin powders or pastes of examples 2 to 2
From the above experimental analysis, the performance of example 2-1 and example 2-2 is inferior compared to example 2-3, example 2-4, and example 2-5, indicating that X, A, B is better when it is the same hydrolytic group. Additionally, examples 2-6 performed better than examples 2-5 and examples 2-10, indicating that R 1 The performance is better when the group is vinyl. In the above table, the experimental examples 2-6 best meet the application requirements.
The group of embodiments provides a modified tin powder, which comprises tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the raw material of the first adhesion layer comprises a disilane compound, and the disilane compound is condensed to form a silane compound containing a silicon-oxygen group so as to form the first adhesion layer. The tin powder particles also comprise a second adhesion layer, the outer surface of the first adhesion layer is coated with the second adhesion layer, and the second adhesion layer is a polymer containing amide groups.
Table 4 shows specific chemical compositions of the starting materials of the first adhesive layer and the monomers corresponding to the amide group-containing polymer in the second adhesive layer in each example of example group 3.
Table 4 shows the chemical composition of the monomer compounds of the first and second adhesive layers in example set 3
The preparation method of the modified tin powder comprises the following steps:
s1, cleaning tin powder particles to obtain first tin powder particles; wherein, no. 7 tin powder is adopted, and is dried after primary acid washing, secondary acid washing and water washing in sequence.
S2, mixing 8 parts of monosilane compound, 90 parts of absolute ethyl alcohol and 2 parts of water according to parts by weight to prepare a first mixed solution; wherein the first mixture in comparative example 3 was only 90 parts absolute ethanol and 2 parts water;
and S3, adding 5g of the first tin powder particles into 200mg of the first mixed solution, stirring for 2h, and drying at 50 ℃ to obtain the modified tin powder.
And S4, adding the first modified tin powder into the amide group-containing polymer, stirring for 2 hours, and drying at 50 ℃ to obtain a finished product.
And finally, adding an auxiliary agent and a soldering flux into the modified tin powder, wherein the auxiliary agent is ethyl acetate to prepare the tin paste, the modified tin powder accounts for 85% of the total mass of the tin paste, and the mass ratio of the modified tin powder to the auxiliary agent is 40:0.5.
the modified solder powders or solder pastes obtained in examples 3-1 to 3-4 and comparative example 3 were tested, and the test items and methods refer to example group 1, and the test results are shown in table 5:
table 5 shows the results of the property tests of the modified solder powder or solder paste obtained in example 3
As is clear from the above test results, the test results of examples 3-4 and 3-3 are superior to those of examples 3-1 and 3-2, indicating that R is the same as R 7 And when the modified tin powder is alkyl hydroxyl or alkyl ether, the bonding force between the modified tin powder and other components in the tin paste is favorably improved.
In summary, the modified tin powder provided by the invention includes tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the first adhesion layer is a silane compound containing a siloxy group. The first adhesion layer can reduce the oxidation of the tin powder before the preparation of the tin paste, and improve the use reliability of the tin paste. In addition, the first adhesion layer can improve the surface performance of the tin powder particles, improve the dispersion capacity of the tin powder particles in the tin paste and reduce agglomeration. In addition, when the first adhesion layer containing a siloxane-based silane compound is formed, curing shrinkage occurs, and additional stress is generated on the surface of the tin powder particles, thereby securing the degree of bonding between the first adhesion layer and the tin powder particles.
Furthermore, the tin powder particles also comprise a second adhesion layer outside, the second adhesion layer is coated on the outer surface of the first adhesion layer, and the second adhesion layer is a polymer containing amide groups. The second adhesion layer enables the modified tin powder and the soldering flux to appropriately coexist, and further meets the application characteristics of the tin paste. The second adhesion layer is a polymer containing amide groups, and a large number of amide groups can form chemical bonds with various components in the soldering flux through nucleophilic or adsorption action, even form hydrogen bonds with macromolecular compounds in the soldering flux, and serve as bridges for tin powder and soldering flux solution, so that the dispersibility of the tin powder in tin paste is improved.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (8)
1. The modified tin powder is characterized by comprising tin powder particles and a first adhesion layer coated on the surfaces of the tin powder particles, wherein the raw materials of the first adhesion layer comprise a disilane compound and a monosilane compound, and the disilane compound and the monosilane compound are subjected to condensation polymerization to form a silane compound containing a siloxy group so as to form the first adhesion layer;
the molecular structural formula of the monosilane compound is (I):
the molecular structural formula (I) is as follows:
the molecular structural formula of the bis-silane compound is (II), (III) or (IV):
the molecular structural formula (II) is as follows:
the molecular structural formula (III) is as follows:
the molecular structural formula (IV) is as follows:
wherein, R is 1 、R 2 Or R 3 Is one of alkyl group, alkenyl group, phenyl group, amino group, halogen group, sulfhydryl group and hydrogen group;
the X is one of alkoxy, halogen group, acyloxy and amino;
a is one of alkyl, alkoxy, halogen group, acyloxy and amino;
b is one of alkyl, alkoxy, halogen group, acyloxy and amino;
m≥0，n≥0。
2. the modified tin powder of claim 1, wherein R is 1 Is an alkenyl group;
and/or, the X, A and B are both alkoxy;
and/or m is more than or equal to 0 and less than or equal to 10,0 and less than or equal to 10.
3. The modified tin powder of claim 2, wherein the X, A, B are of the same molecular structure;
and/or the alkoxy is one or more of methoxy, ethoxy, propoxy and isopropoxy;
and/or m is more than or equal to 1 and less than or equal to 3,1 and less than or equal to 3.
4. The modified tin powder of claim 1, further comprising a second adhesion layer over the tin powder particles, the second adhesion layer coating an outer surface of the first adhesion layer, the second adhesion layer being a polymer comprising an amide group.
5. The modified tin powder of claim 4, wherein the second adhesion layer has a molecular structure of (V):
the molecular structural formula (V) is:
wherein, R is 4 、R 5 Or R 6 Is one of hydrogen radical or alkyl;
said R is 7 In hydrogen, alkyl, hydroxyl, ether, phenylOne or more of;
the above-mentionedl≥3。
6. The modified tin powder of claim 5, wherein R is 7 Is alkyl hydroxyl or alkyl ether;
and/or, 5 is less than or equal tol≤15。
7. A process for preparing a modified tin powder according to any one of claims 4 to 6, characterized in that it comprises the following steps:
cleaning the tin powder particles to obtain first tin powder particles;
mixing a monosilane compound and a disilane compound with an alcohol substance and water to prepare a first mixed solution;
adding the first tin powder particles into the first mixed solution, stirring for a preset time, and drying to obtain first modified tin powder;
and adding the first modified tin powder into the polymer containing the amide group, stirring for a preset time, and drying to obtain a finished product.
8. A solder paste comprising the modified solder powder of any one of claims 1 to 6 and a flux.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3137462B2 (en) * | 1992-10-21 | 2001-02-19 | トヨタ自動車株式会社 | Cream solder |
| JPH0919794A (en) * | 1995-07-03 | 1997-01-21 | Showa Denko Kk | Powdered solder |
| US6331329B1 (en) * | 1999-05-17 | 2001-12-18 | University Of Massachusetts | Surface modification using hydridosilanes to prepare monolayers |
| JP2004339583A (en) * | 2003-05-16 | 2004-12-02 | Sony Corp | Surface treatment agent for tin or tin alloy material, tin or tin alloy material, surface treatment method therefor, tin alloy based solder material, solder paste obtained by using the same, method of producing tin alloy based solder material, electronic component, printed circuit board and mounting structure for electronic component |
| CN102146091B (en) * | 2011-01-26 | 2013-12-04 | 湖北德邦化工新材料有限公司 | Bis-silane coupling agent and preparation method thereof |
| JP6160498B2 (en) * | 2013-03-08 | 2017-07-12 | 住友金属鉱山株式会社 | Coated solder material and manufacturing method thereof |
| CN111660037B (en) * | 2019-03-05 | 2022-04-15 | 潮州三环（集团）股份有限公司 | Soldering flux and solder paste containing same |
| CN111872599B (en) * | 2020-07-01 | 2022-02-22 | 潮州三环（集团）股份有限公司 | Modified tin powder and tin paste |
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