You didn't indicate what rule set you are using so I will give an answer using USAV and NFHS rules.
I don't have my NFHS rule book in front of me but I am pretty sure that there is no delay of game penalty unless this is a pattern of that team. If I saw a player standing in the substitution zone after I whistled for serve, I would stop play, send the player back to the bench, and issue a re-serve. Some coaches like to wait until the last possible instant to send in the sub (hoping that will disrupt the server's concentration) and the officials sometimes will not notice until after the signal for service. If this causes more than one delay in a match, I will warn the coach that if this continues I will call a delay of game penalty. That would not be a yellow card but the offending team would be charged with a time out. If they had used both time outs already, they would be charged with a loss of rally.
USAV rules are different. According to rule 20.7.1 this would be an improper request. No penalty other than a notation on the scoresheet. If the offending team already has been charged with an improper request in that game, it is a team delay warning. Again, a notation on the scoresheet but no penalty. Only if the team has already been charged with a team delay warning in the same game is there a penalty (yellow card held against wrist=loss of rally).
Just as a side note, a yellow card in NFHS rules is a warning with no loss of rally. In USAV rules, a yellow card does constitute a loss of rally penalty.
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